Manufacturing .
There are two main way to Manufacturing of Phenobarbital.
It is prepared from benyl cyanide.
Barbiturate drugs are obtained via condensation reactions between a derivative of diethyl malonate and urea in the presence of a strong base.
Here we Phenobarbital prepared from benyl cyanide.
1. Chemical Process Industries - 2
(2140506)
TOPIC
Manufacturing of Phenol Barbital
Presented by
Rana Pranav (160170105046)
Rathava Atul (160170105047)
Savukiya Ankit (160170105048)
Shah Subham (160170105049)
2. INTRODUCTION
PROPERTIES PARTICULAR
Chemical Name Phenobarbital , phenobarbitone , luminal ,
5-Ethyl-5-pheny1-1,3-diazinane-2,4,6-trione
Structure
Molecular Formula C12H12N2O3
Molecular Weight 232.2 gm/mole
Appearance Crystalline powder or colorless crystal
Odor Odorless
Solubility Insoluble in water and benzene; soluble in ethanol, ethyl ether;
slightly soluble in dimethtyl sulfoxide
Melting point 174 ⁰C
3. Manufacturing
There are two main way to Manufacturing of
Phenobarbital.
1. It is prepared from benyl cyanide.
2. Barbiturate drugs are obtained
via condensation reactions between
a derivative of diethyl malonate and urea in
the presence of a strong base.
• Here we Phenobarbital prepared from benyl
cyanide.
4. Raw Materials:
Benyl Cyanide , Ethanol , Diethyl carbonate ,
Sulfuric acid, Ethyl bromide, Urea
Chemical reaction:-
It is Prepared from benyl cyanide by following
steps:
6. Process Description
Preparation of Diethyl phenyl ethyl malonate : in reflux kettle
with jacket and agitator, clean sodium metal is taken and
dissolved it in absolute ethanol to prepare sodium ethylate
solution.
Diethyl carbonate is charged with stirring and dissolve it in
sodium ethylate solution.
Benzyl cyanide is added drop wise to a solution and reflux the
reaction mixture for 5 hours.
It is them cooled, collected from bottom of kettle and charged
into another jacketed reflux kettle.
Cooled mixture of sulfuric acid in anhydrous ethanol is added.
This alcoholic mixture is refluxed for 5 hrs and cooled.
7. The reaction mass is collected from bottom and transferred
into neutralization chamber.
Sodium ethylate is charged with stirring to precipitate
sodium sulphate.
The mass undergo filtration to remove sodium sulphate.
The filtration is added into jacketed reflux kettle containing
sodium metal.
Reflux while adding ethyl bromide drop wise.
Heat for another 2 hrs after the addition is completed .
Remove the alcohol by distillation and dissolve the remaining
residue in water.
Extract the substance from the water with benzene and
vacuum distillation to get pure diethyl phenyl malonate and
benzenes is recycled.
8. Preparation Of Phenobarbitone :
Pure diethyl phenyl ethyl malonate and dry urea are stirred
together in a vessel equipped with an efficient stirring device.
To the above mixture add a solution of clean metallic sodium
in dry ethanol.
Heat to boiling and distill the ethanol off slowly, over six hrs
with stirring.
When the alcohol is completely distilled out of the mixture,
the remaining white powder is added to hydrolysis chamber.
Coned hydrochloric acid in water and finely crushed ice is
added in chamber.
The mixture is kept at 0 ⁰C until the acid has crystallized,
then it is centrifuged and give charcoal treatment to get pure
phenobarbitone.