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Experiment No: - 1
Experiment No: - 1
PROCEDURE: - Add dry acetanilide (25 g) to glacial acetic acid (25 ml) in a beaker
and then introduce concentrated sulphuric acid (50 ml) slowly with constant stirring
to obtain clear solution. Place the beaker in a freezing mixture of ice and salt to cool
the solution below 5 oC. Add a cold mixture of concentrated nitric acid (11 ml) and
concentrated sulphuric acid (7 ml) drop wise with constant stirring to a reaction
mixture while maintaining the temperature below 5 oC. After adding all the mixed
acid, remove the beaker from the freezing mixture and keep it for 1 hr at room
temperature. Pour the reaction mixture into an ice cold water (30 ml) to obtain the
crude product of p-nitroacetanilide. Filter it on suction, wash with cold water till free
from acid and recrystallize the pale yellow product from ethanol to get colourless
crystalline solid, m.p. 2145 oC.
NOTE: - o-Nitroacetanilide remains in the filtrate due to its more solubility in water.
EXPERIMENT No: - 2
Date: AIM: - Synthesis of Benzillic acid from Benzoin.
REAGENTS: - Benzoin, Glacial acetic acid, Conc. HNO3,
Benzil, KOH, Methanol, Conc, H2SO4
REACTION: - Step 1
OH O
C
HNO3
H
Benzoin
Step 2
Benzil
O
C
O
C
OH OK
KOH
C
O
HCl
OH OH
C
C
O
Benzilic acid
PROCEDURE: Step 1: - Heat a mixture of benzoin (1 g), glacial acetic acid (5 ml) and conc. nitric acid
(25 ml) in a test tube on boiling water bath for one hour. Then, pour down the
contents into ice cold water (50 ml) with continuous shaking. Filter the product,
wash the solid with cold water, and recrystallize from methanol, m.p. 92 oC.
Step 2: - Dissolve KOH (7 g) in water (15 ml) by heating on hot plate and the cool to
room temperature. Disolve benzyl (7 gm) in methanol by heating on a water bath for
15 minutes. Cool down the contents and pour into alkali solution with stirring.
Reflux the content on a water bath till blue colour disappears. Cool in ice, collect the
colorless needles pot. Benzillate. Dissolve the solid in minimum quantity of hot
water and acidify with HCl. Collect the solid benzillic acid and recrystallize from
ethanol.
EXPERIMENT No: - 7
Date: AIM: - Synthesis of Chalcone (1, 3-diphenylprop-2-en-1- one) from Bendzaldehyde
and Acetophenone.
REAGENTS: - Bendzaldehyde, Acetophenone, NaOH, Rectified spirit
REACTION: -
O
O
CH3
NaOH
Benzaldehyde
Acetophenone
Chalcone
EXPERIMENT No: - 8
Date: AIM: - Synthesis of Barbituric acid from Urea and Dimethyl malonate.
REAGENTS: - Urea, Dimethyl malonate, Sodium metal, Absolute Ethanol
REACTION: -
O
H2 N
EtO
OEt
NH
O
O
Diethyl malonate
OEt
H2 N
Urea
N
H
Barbituric acid
PROCEDURE: - In a 2-litre round bottomed flask, fitted with a double surface reflux
condenser, place 11.5 g (0.5 mol) of clean sodium. Add 250 ml absolute ethanol in one
portion: if the reaction is unduly vigorous, immerse the flask momentarily in ice. When
all the sodium has reacted, add 80 g (76 ml, 0.5 mol) of diethyl malonate, followed by a
solution of 30 g (0.5 mol) of dry urea in 250 ml of hot (about 70C) absolute ethanol.
Shake the mixture well, fit a calcium chloride guard-tube to the top of the condencer and
reflux the mixture for 7 hours in an oil bath heated to 110C. A white solid separates.
Treat the reaction mixture with 450 ml of hot (50C) water and then with concentrated
hydrochloric acid, with stirring, until the solution is acidic (about 45 ml). Filter the
resulting almost clear solution and leave it in the refrigerator overnight. Filter the solid at
pump, wash it with 25 ml of cold water, drain well and then dry at 100C for 4 hours. The
yield of barbituric acid is 50 g (78%). It melting point of product is 245C.