ORGANIC PREPARATION SEM-II

Preparation Of β-Resorcylic Acid From Resorcinol

Aim:- Organic Preparation Of β-Resorcylic Acid
Requirement:-Resorcinol, K2CO3, dil. HCl, NaHCO3, Conc. HCl, H2O, Reflux Condenser,
Gas Inlet Tube
Procedure:-
Place A Solution Containing 10 gms of Resorcinol, 50 gms of NaHCO3 & 100 ml of H2O in
a 250 ml R.B.F fitted with a reflux condenser & gas inlet tube heat it on a water bath for
about one hour then reflux vigorously over a flam on wire gauge for 30 min. passing a
rapid stream of CO2 through the soln.[about 15 to 20 min]
Acidify the soln. while still hot by adding conc. HCl. Allow to cool to room temp. chill in an
ice bath and collect the crude β-Resorcylic Acid by filtration.
Recrystallize the product by boiling water in present of a little decolorizing carbon filter
and cool in an ice salt mixture with stirring collect and dry the pure β-Resorcylic Acid
Theoretical Yield=14.0gms
M.P.:-216-217 oC
Reaction:-

OH OH

NaHCO3

OH OH

Resorcinol COOH
-Resorcylic Acid

Calculation:-
110 gms Resorcinol gives 154 gms β-Resorcylic Acid
10 gms Resorcinol gives (?) gms β-Resorcylic Acid

= = 14.0 gms β-Resorcylic Acid

Theoretical Yield=14.0gms
Practical Yield = _________ gms

% Yield =
 ORGANIC PREPARATION SEM-II

Preparation Of Resacetophenone From Resorcinol

Aim:- Organic Preparation Of Resacetophenone
Requirement:-Resorcinol, Anhydrous ZnCl2, Glacial HAc, 50% HCl
Procedure:-

Take 10 gms resorcinol & heat the mixture on a sand bath until it just begins to boil. Now
allow the reaction to complete itself on sand bath without further heating for half hour.

Cool the reaction mixture and dilute it with 50% HCl[about 2 to 3 T.T] keep it for some
times & shake it well Resacetophenone slowly separate from the solution in orange need
filters it & wash water & dry it. Recrystallized it from the boiling water.

Theoretical Yield=13.8 gms

M.P.:-144-147 oC
Reaction:-

OH OH

CH3COOH
ZnCl 2
-H2O
OH OH

COCH3

Calculation:-
110 gms Resorcinol gives 152 gms Resacetophenone
10 gms Resorcinol gives (?) gms Resacetophenone

= = 13.8 gms Resacetophenone

Theoretical Yield=14.0 gms

Practical Yield = _________ gms

% Yield =
 ORGANIC PREPARATION SEM-II

Preparation Of Benzimidazole From o-phenylene diamine

Aim:- Organic Preparation Of Benzimidazole
Requirement:- o-phenylene diamine, 90% Formic acid, 10% NaOH, Ice
Procedure:-
Take 10gms of o-phenylene diamine in 250 ml R.B.F & 6 ml of 90% Formic acid. Heat the
mixture on a water bath at 100 oC for 2 hours cool the flask & then add 10% NaOH soln.
slowly with constant rotation of the flask until the mixture is just alkaline [check on litmus
paper] filter off the crude Benzimidazole at the pump & wash with ice cold water for
recrystallization, dissolve the crude product in about 150 ml of water boil it & add 75 gms
of decolorizing carbon & digest for 15 minutes. Filter rapidly at the pump cool the filtrate
to about 10 oC filter off the Benzimidazole wash with cold water & dry at 100 oC.
Theoretical Yield=10.93 gms

M.P.:-171-172 oC
Reaction:-

NH2 H
N
2 Hrs
H-COOH CH

-2H2O N
NH2

O-phenylene diamine Formic acid Benzimidazole

Calculation:-
108 gms O-phenylene diamine gives 118 gms Benzimidazole
10 gms O-phenylene diamine (?) gms Benzimidazole

= = 10.93 gms Benzimidazole

Theoretical Yield=14.0 gms

Practical Yield = _________ gms

% Yield =
 ORGANIC PREPARATION SEM-II

Preparation Of 4-Methyl-7-Hydroxy Coumarin From Resorcinol

Aim:- Organic Preparation Of 4-Methyl-7-Hydroxy Coumarin
Requirement:- 15 ml Conc. H2SO4, 3.7 gms Resorcinol, 5 ml Ethyl Acetoacetate, NaOH &
HCl
Procedure:-

15 ml Conc. H2SO4 in a wide necked 50 ml flask cool it. Externally till the temp. of the acid
is about 5 oC mean while prepare a solution of Resorcinol [3.7 gms to 4.0 gms] in 4.4 ml of
Ethyl acetoacetate.

Now add the solution of Resorcinol in Ethyl Acetoacetate to Conc H2SO4 slowly. So that the
temp of mixture does not rise about 10 oC continue the stirring for 30 minutes. Pour the
mixture into crushed ice when the solid separates. Filter of the Coumarin at the pump. .
Recrystallized it from Alcohol

Theoretical Yield=6.40 gms

M.P.:-188-190 oC
Reaction:-
OH C2 H5 O
O
C HO O O

CH 2
Conc. H2SO4

C
OH H3 C O
CH 3
Resorcinol Ethyl Acetoacetate 4-Methyl-7-Hydroxy Coumarin

Calculation:-
110 gms Resorcinol gives 176 gms 4-Methyl-7-Hydroxy Coumarin
4.0 gms Resorcinol (?) gms 4-Methyl-7-Hydroxy Coumarin
.
= = 10.93 gms 4-Methyl-7-Hydroxy Coumarin

Theoretical Yield=6.4 gms

Practical Yield = __________ gms

% Yield =
 ORGANIC PREPARATION SEM-II

Preparation Of Methyl Orange From Sulphanilic Acid

Aim:- Organic Preparation Of Methyl Orange
Requirement:- Sulphanilic Acid, Anhydrous Na2CO3, NaNO3, NaCl, Dimethyl Aniline,
20% NaOH, ice etc.
Procedure:-
in a 250ml beaker take 5.0 gms of Sulphanilic acid, 1.5 gm of Anhydrous Na2CO3 & 50 ml
of water and warm until a clear solution is obtained cool the soln. under the tap to about 15
o
C & then place it in a ice bath. Now add this cold soln. of NaNO3 into a cold solution of
Sulphanilic Acid. Slowly with constant stirring.
Now pour this resulting solution slowly & with stirring into a 500 ml beaker containing 5
ml of Conc. HCl & 30 gms Crushed ice.
Stir well this mixture for 10 min &maintain the temp. Below 10 oC using the ice bath.
Diazobenzene sulphonate will soon separate out. Do not filter this off as they will dissolve
during the next stage of preparation.
Now dissolve 3.0 ml of Dimethyl Aniline into cold soln. of diazotized Sulphanilic acid with
constant stirring. Allow the mixt. To stand for 10 min the red or acid form of methyl
Orange will gradually separated.
After 10 min add slowly & with stirring 25 ml of 20% NaOH soln. the mixture will assume
a uniform Orange color due to separation of the sodium salt of Methyl Orange in fine
particles.[add NaOH till Alkaline]

Now heat the contents almost to boiling stage & add 5.0gms of NaCl & again warm it at 80-
90 oC. Until the salt has dissolved completely.

Allow the mixture to cool undisturbed for 15 min & then cool it in ice bath. Filter the
product wash with water & recrystallized it from hot water.

Theoretical Yield=6.40 gms

M.P.:-Not well defined

Reaction:-

NH2 N=N

N=N N(CH 3) 2

Diazotization coupling Rean.

NaNO2+HCl
N(CH 3)2
0-5 oC
Dimethyl aniline
SO3 Na
SO 3H SO 3H
Methyl Orange
 ORGANIC PREPARATION SEM-II

Calculation:-
173 gms Sulphanilic Acid gives 327 gms Methyl Orange
5.0 gms Sulphanilic Acid (?) gms Methyl Orange
.
= = 9.45 gms Methyl Orange

Theoretical Yield=9.45 gms

Practical Yield = __________ gms

% Yield =

Preparation Of P-Nitro Aniline From Acetanilide

Aim:- Organic Preparation Of P-Nitro Aniline
Step 1:- Acetanilide to P-Nitro Acetanilide [Nitration]
Requirement:- powdered Acetanilide (dry), Glacial HAc, Conc. H2SO4, ice, Fuming HNO3,
Alcohol
Procedure:-
Take 10 gms of powdered Acetanilide (dry) & 15 ml Glacial HAc in a 250ml beaker & add
20 ml of Conc. H2SO4 with stirring the mixture becomes warm and clear solution is
obtained.
Surround the beaker with freezing mixture of ice & salt and stir the solution mechanically
Now, take 5 ml fuming HNO3 & 3 ml Conc. H2SO4 in a 100 ml beaker cool the acid solution
& transfer it in a separating funnel.
When the temp. of the solution from separating funnel drop by drop and maintain the tem
below 10 oC.
When all the mixed acid has been added remove the beaker from the freezing mixture and
allow it to stand at room temperature for at least about 1 hour and then pour the reaction
mixture into an ice containing water.
Crude P-Nitro Acetanilide is at once precipitated allow it to stand for 15 min. filter the
product, wash it with cold water till free from acids[checks on litmus paper] dry it.
Recrystallized the product with alcohol.
Theoretical Yield=13.3 gms

M.P.:- 214 oC
 ORGANIC PREPARATION SEM-II

Reaction:-
NHCOCH 3
NHCOCH 3

Cold Mixture
Fuming HNO3 + Conc. H2SO4

Glacial HAc
0 - 10 oC
Acetanilide
NO2
P-Nitro Acetanilide

Calculation:-
135 gms Acetanilide gives 180 gms P-Nitro Acetanilide
10 gms Acetanilide (?) gms P-Nitro Acetanilide

= = 13.3 gms P-Nitro Acetanilide

Theoretical Yield=13.3 gms

Practical Yield = __________ gms

% Yield =

Step 2:- P-Nitro Acetanilide to P-Nitro Aniline [Acid Hydrolysis]

Requirement:- P-Nitro Acetanilide, 70% Conc. H2SO4[60ml Conc. H2SO4+45 ml H2O],
10% NaOH or Conc. Ammonia Solution.
Procedure:-
Take 10 gm P-Nitro Acetanilide & 50 ml of 70% Conc. H2SO4 in a 250ml R.B.F attach a
reflux condenser & reflux it for about half hour [or until a test sample remains clear upon
dilution with 2 – 3 times its volume with water]
The P-Nitro Aniline is present in the liquid as sulphate. Pour the clear hot solution into
cold water and precipitate the P-Nitro Aniline by adding excess of Conc. Ammonia
solution. Cool the mixture in ice water.
Filter the yellow crystalline P-Nitro Aniline. Wash with water & dry it. Recrystallize the
product with hot water.
Theoretical Yield=7.6 gms

M.P.:- 147 oC
 ORGANIC PREPARATION SEM-II

Reaction:-
NHCOCH 3 NH2

Acid Hydrolysis
CH3COOH

NO2 NO2
P-Nitro Acetanilide P-Nitro Aniline

Calculation:-
180 gms P-Nitro Acetanilide gives 138 gms P-Nitro Aniline
10 gms P-Nitro Acetanilide (?) gms P-Nitro Aniline

= = 13.3 gms P-Nitro Aniline

Theoretical Yield=7.6 gms

Practical Yield = __________ gms

% Yield =

Preparation Of P-Bromo Aniline From Acetanilide

Aim:- Organic Preparation Of P-Bromo Aniline
Step 1:- Acetanilide to P-Bromo Acetanilide [Bromination]
Requirement:- powdered Acetanilide (dry), Glacial HAc, Bromine, ice, NaHSO3
Procedure:-
Take 5 gms of finely powdered Acetanilide in 15 ml of glacial HAc in R.B.F & cool it in ice
bath in another 100 ml beaker take 3 ml of bromine & dissolve it in 12 ml of HAc &
transfer the solution slowly and with constant shake to cold solution of acetanilide which is
preserved in ice bath when all the bromine has been added the solution will turn an orange
due to the slight excess of bromine. All the reaction mixture into ice cold water in a 500 ml
beaker stir the mixture and add just sufficient NaHSO3 solution to remove the orange
color. Filter the product, wash with ice cold water and dry it. Recrystallized the product
with Alcohol.
Theoretical Yield=15.8 gms

M.P.:- 167 oC
 ORGANIC PREPARATION SEM-II

Reaction:-
NHCOCH 3 NHCOCH 3

Bromination

Br2 in Glacial HAc

Acetanilide
Br
P-Bromo Acetanilide

Calculation:-
135 gms Acetanilide gives 214 gms P-Bromo Acetanilide
5 gms Acetanilide (?) gms P-Bromo Acetanilide

= = 7.92 gms P-Bromo Acetanilide

Theoretical Yield=7.92 gms

Practical Yield = __________ gms

% Yield =

Step 2:- P-Bromo Acetanilide to P-Bromo Aniline

Requirement:- P-Bromo Acetanilide, Ethanol, KOH(solid), ice
Procedure:-
Take 7 gms P-Bromo Acetanilide & 15 ml Ethanol in a 250 ml R.B.F attached a reflux
condenser & heat the mixture till a clear solution is obtained [if necessary add more
alcohol]
Meanwhile prepare a solution of 4 gms KOH in 10 ml of waters. Add this solution in a clear
soln. of R.B.F & reflux the contents for about 2 hours. Cool & add the contents of the flask
in a 250 ml beaker containing 100 ml ice cold water. The precipitate of P-Bromo Aniline is
obtained. Filter the product and dry it. Recrystallized the product with rectified sprite.
Theoretical Yield=5.6 gms

M.P.:- 66.6 oC
 ORGANIC PREPARATION SEM-II

Reaction:-
NHCOCH 3 NH2

Alkiline Hydrolysis

KOH

Br
Br
P-Bromo Acetanilide P-Bromo Aniline

Calculation:-
214 gms P-Bromo Acetanilide gives 172 gms P-Bromo Aniline
7 gms P-Bromo Acetanilide (?) gms P-Bromo Aniline

= = 5.6 gms P-Bromo Aniline

Theoretical Yield=5.6 gms

Practical Yield = __________ gms

% Yield =

Result:-

Step Product Theoratical Practical % of Structural Formula M.P

Yield Yield Yield
 β Resorcylic Acid
Reaction:

Mechanism:
 Resacetophenone
Reaction:

Mechanism:

OH OH
OH

CH3CO
OH - O H
OCH3C H
O

OH

OH

COCH3
 o-Phenylene Diamine
Reaction:

Mechanism:
 4-Methyl-7-Hydroxy Coumarin
Reaction:

Mechanism:
 Methyl Orange
Reaction:

Mechanism:

H N H H N H H N N O H N N O H

Na2CO3 Diazotization Proton -H2O

-NaHCO3 NaNO2+2HCl Shift
0 - 5 oC
+NO
SO3H SO3Na SO3Na SO3Na

N N N N Cl

+Cl

SO3Na SO3Na
 CH3
N N Cl N CH3
CH3
N N N

HCl CH3

SO3Na H

SO3Na

CH3

N N N

CH3

Methyl Orange
SO3Na

P-Nitro Aniline
Step 1:- Acetanilide to P-Nitro Acetanilide [Nitration]

Reaction:

Mechanism:
 NHCOCH3 NHCOCH3 NHCOCH3 NHCOCH3

H H NO2
NO2

Step 2:- P-Nitro Acetanilide to P-Nitro Aniline [Acid Hydrolysis]

Reaction:-
NHCOCH3 NH2

Acid Hydrolysis
CH3COOH

NO2 NO2
P-Nitro Acetanilide P-Nitro Aniline

Mechanism:
 P-Bromo Aniline
Step 1:- Acetanilide to P-Bromo Acetanilide [Bromination]
Reaction:

Mechanism:

Step 2:- P-Bromo Acetanilide to P-Bromo Aniline

Reaction:
Mechanism:
 ORGANIC ESTIMATION SEMESTER-II

Determine the % purity of Formaldehyde

Aim:- to determine the % purity of Formaldehyde by Hydroxyl Amine Hydrochloride Method
Requirement:- Formaldehyde, 10 % Hydroxyl Amine Hydrochloride soln., Exact 0.1N NaOH
soln., Bromo phenol blue Indicator
Process:-
1. Blank Experiment:-
Take 25 ml of distilled H2O in a conical flask. Add about 1 ml Bromo phenol blue
Indicator & then add 10 ml soln. of 10 % Hydroxyl Amine Hydrochloride & titrate it
against 0.1N NaOH soln. from the burrete yellow soln. changes to blue violet is the end
point. Take 3 to 4 readings. Let the constant burrete reading “V2” ml.
2. Actual Experiment:-
Weight out accurate about 0.270 to 0.300 gms of the given formaldehyde soln. in a
weighting bottle. Transfer it to a conical flask by 25 ml dist. H2O. then add about 1 ml
Bromo phenol blue Indicator & then add 10 ml soln. of 10 % Hydroxyl Amine
Hydrochloride &allow to stand for 10 min & shake frequently. Then titrate the liberated
Hydrochloride acid against 0.1N NaOH soln. from the burrete yellow soln. changes to
blue violet is the end point. Take 3 to 4 readings.let the constant burrete reading “V 1” ml.
Reaction:-

Observation:-Blank Estimation:-
Burette:- 0.1N NaOH Soln.
Flask:- 10 ml 10 % Hydroxyl Amine Hydrochloride + 25 ml dist. H2O
Indicator:- Bromo phenol blue Indicator
End point:- yellow to blue colour

No. I.B.R F.B.R Difference Mean

1 0.0 ml
2 0.0 ml
3 0.0 ml

Observation:-Actual Estimation:-
Burette:- 0.1N NaOH Soln.
Flask:- weighted formaldehyde soln. + 10 ml 10% Hydroxyl Amine Hydrochloride + 25 ml dist.
H2O
Indicator:- Bromo phenol blue Indicator
End point:- yellow to blue colour

1
 ORGANIC ESTIMATION SEMESTER-II

No. Weighted F.B.R % of purity

1 gms
2 gms
3 gms

Calculation:-
( )
% of HCHO = .
N=0.104
M=30
Result:-
% purity of Formaldehyde:-___________.

Determine the Amount of Acid + Amide

Aim:- you are given a mixed solution of acid & amide. Determine the amount of acid & amide in
the given solution.

Requirement:- 0.1N HCl (exact), 0.1N NaOH (exact), 1.5N NaOH (approx.), phenolphthalein
indicator

Process:-Blank estimation:-[standardization of NaOH]

Take 25 ml of 1.5N NaOH in a 250 ml S.M.F & diluted it to 250 ml with dist. H 2O. take 25 ml of
the diluted soln. in a conical flask & titrate it against 0.1N HCl soln. from burette using
phenolphthalein as an indicator disappearance of pink color is the end point. Take 3 or 4 reading.
Let the constant burette reading “A” ml.

Estimation of Acid:-
Take 25 ml of given mixed soln of acid+amide in a 250 ml S.M.F & dilute it to 250 ml dist. H 2O.
Take 25 ml of this diluted soln.in a conical flask and titrate it against 0.1N NaOH soln. from
burette using phenolphthalein as an indicator. Appearance of pink color is the End point. Take 3
to 4 burette reading. Let the constant burette reading “D” ml.

Actual Estimation [Estimation of Acid + Amide]:-

Take 25ml of given mixed soln. of acid + amide in 250 ml R.B.F. add exact 25 ml of 1.5 N
NaOH by pipette & 2 to 3 T.T dist. H2O attach on air condenser & refluxed the content on a sand
bath. Cool the content & transfer the Hydrolyzed.
Take 25 ml this diluted Hydrolyzed soln. in a conical flask & titrate it against 0.1N HCl soln.
from burette using phenolphthalein as an indicator. Disappearance of pink color is the end point.
Take 3 to 4 reading. Let the constant burette reading. Let the burette reading “B” ml.

2
 ORGANIC ESTIMATION SEMESTER-II

Observation: Blank estimation [standardization of NaOH soln.]

Burette:- 0.1N HCl Soln.
Flask:- 25 ml dil. Soln. of NaOH
Indicator:- phenolphthalein Indicator
End point:- disappearance of pink color

No. I.B.R F.B.R Difference Mean

1 0.0 ml
2 0.0 ml
3 0.0 ml

25ml diluted NaOH soln. required (A)=_____ml 0.1N HCl.

.
Normality of given NaOH soln.= 10
=__________ N

Estimation of Acid:-
Burette:- 0.1N NaOH Soln.
Flask:- 25 ml dil. Soln. of [Acid + Amide]
Indicator:- phenolphthalein Indicator
End point:- Appearance of pink color

No. I.B.R F.B.R Difference Mean

1 0.0 ml
2 0.0 ml
3 0.0 ml
25 ml diluted solution Reqn. D =_________ ml 0.1 N NaOH

Reaction:-

Calculation:-

1000 ml 1 N NaOH = 59 gms Succinic Acid

1 ml 0.1 N NaOH = 0.0059 gms Succinic Acid
D ml 1 N NaOH = 0.0059 X D gms Succinic Acid
E = _______ gms Succinic Acid

Amount of succinic acid in 25 ml diluted solution E = ________ gms

Amount of succinic acid in given solution = E X 10
X = ________ gms
3
 ORGANIC ESTIMATION SEMESTER-II

Actual estimation [Estimation of Acid + Amide]:-

Burette:- 0.1N HCl Soln.
Flask:- 25 ml dil. Refluxed [Hydrolyzed Soln.]
Indicator:- phenolphthalein Indicator
End point:- Disappearance of pink color

No. I.B.R F.B.R Difference Mean

1 0.0 ml
2 0.0 ml
3 0.0 ml

25 ml diluted refluxed [Hydrolyzed Soln.] required B = _______ ml 0.1 N HCl

Reaction:-

Now,

1. The amt. of NaOH soln. added in terms of 0.1 N HCl A = ______ ml

2. The amt. of NaOH soln. unused in terms of 0.1 N HCl B = ______ ml
3. The amt. of NaOH soln. used up for acid + amide in terms of 0.1 N HCl C = A – B ml
C = ________ ml
4. The amt. of NaOH soln. used up for amide only in terms of 0.1 N HCl F = C – D ml
F = _______ ml
Now,
1000 ml 1 N NaOH = 1000 ml 1 N HCl = 59 gms Acetamide
1000 ml 1 N HCl = 59 gms Acetamide
1 ml 0.1 N HCl = 0.0059 gms Acetamide
F ml 0.1 N HCl = 0.0059 X F gms Acetamide
G = _______ gms Acetamide
Amt. of Acetamide in the given solution = G X 10
Y = ________ gms.
RESULT:-
1. Normality of given NaOH solution = _______ N
2. Amt. of Acid in the given solution = ________ (X) gms
3. Amt. of Amide in the given solution = ________ (Y) gms

4
 ORGANIC ESTIMATION SEMESTER-II

Determine the Amount of Acid + Ester

Aim:- you are given a mixed solution of acid + Ester. Determine the amount of acid & E in the
given solution.

Requirement:- 0.1N HCl (exact), 0.1N NaOH (exact), 1.5N NaOH (approx.), phenolphthalein
indicator

Process:-Blank estimation:-[standardization of NaOH]

Take 25 ml of 1.5N NaOH in a 250 ml S.M.F & diluted it to 250 ml with dist. H2O. take 25 ml of
the diluted soln. in a conical flask & titrate it against 0.1N HCl soln. from burette using
phenolphthalein as an indicator disappearance of pink color is the end point. Take 3 or 4 reading.
Let the constant burette reading “A” ml.

Estimation of Acid:-
Take 25 ml of given mixed soln of acid+Ester in a 250 ml S.M.F & dilute it to 250 ml dist. H 2O.
Take 25 ml of this diluted soln.in a conical flask and titrate it against 0.1N NaOH soln. from
burette using phenolphthalein as an indicator. Appearance of pink color is the End point. Take 3
to 4 burette reading. Let the constant burette reading “D” ml.

Actual Estimation [Estimation of Acid + Amide]:-

Take 25ml of given mixed soln. of acid + ester in 250 ml R.B.F. add exact 25 ml of 1.5 N NaOH
by pipette attach water condenser & reflux it on water bath till hydrolysis is complete [ 1 and half
hour hour].
Cool it and transfer the reflux solution in a 250 ml S.M.F & dilute it to250 ml with dist. H 2O.
Take 25 ml this diluted refluxed soln. in a conical flask & titrate it against 0.1N HCl soln. from
burette using phenolphthalein as an indicator. Disappearance of pink color is the end point. Take
3 to 4 reading. Let the constant burette reading. Let the burette reading “B” ml.

Observation: Blank estimation [standardization of NaOH soln.]

Burette:- 0.1N HCl Soln.
Flask:- 25 ml dil. Soln. of NaOH
Indicator:- phenolphthalein Indicator
End point:- disappearance of pink color
No. I.B.R F.B.R Difference Mean
1 0.0 ml
2 0.0 ml
3 0.0 ml

25ml diluted NaOH soln. required (A)=_____ml 0.1N HCl.

.
Normality of given NaOH soln.= 10
=__________ N

5
 ORGANIC ESTIMATION SEMESTER-II

Estimation of Acid:-
Burette:- 0.1N NaOH Soln.
Flask:- 25 ml dil. Soln. of [Acid + Ester]
Indicator:- phenolphthalein Indicator
End point:- Appearance of pink color

No. I.B.R F.B.R Difference Mean

1 0.0 ml
2 0.0 ml
3 0.0 ml
25 ml diluted solution Reqn. D =_________ ml 0.1 N NaOH

Reaction:-

Calculation:-

1000 ml 1 N NaOH = 60 gms HAc

1 ml 0.1 N NaOH = 0.0060 gms HAc
D ml 1 N NaOH = 0.0060 X D gms HAc
E = _______ gms HAc

Amount of HAc d in 25 ml diluted solution E = ________ gms

Amount of HAc in given solution = E X 10
X = ________ gms

Actual estimation [Estimation of Acid + Amide]:-

Burette:- 0.1N HCl Soln.
Flask:- 25 ml dil. Refluxed Soln.
Indicator:- phenolphthalein Indicator
End point:- Disappearance of pink color

No. I.B.R F.B.R Difference Mean

1 0.0 ml
2 0.0 ml
3 0.0 ml

6
 ORGANIC ESTIMATION SEMESTER-II

25 ml diluted refluxed Soln. required B = _______ ml 0.1 N HCl

Reaction:-

Now,

1. The amt. of NaOH soln. added in terms of 0.1 N HCl A = ______ ml

2. The amt. of NaOH soln. unused in terms of 0.1 N HCl B = ______ ml
3. The amt. of NaOH soln. used up for acid + ester in terms of 0.1 N HCl C = A – B ml
C = ________ ml
4. The amt. of NaOH soln. used up for ester only in terms of 0.1 N HCl F = C – D ml
F = _______ ml
Now,
1000 ml 1 N NaOH = 1000 ml 1 N HCl = 88 gms Ethyl acetate
1000 ml 1 N HCl = 88 gms Ethyl acetate
1 ml 0.1 N HCl = 0.0088 gms Ethyl acetate
F ml 0.1 N HCl = 0.0088 X F gms Ethyl acetate
G = _______ gms Ethyl acetate
Amt of Ethyl acetate in the given solution = G X 10
Y = ________ gms.
RESULT:-
5. Normality of given NaOH solution = _______ N
6. Amt. of Acid in the given solution = ________ (X) gms
7. Amt. of Ester in the given solution = ________ (Y) gms