Manufacturing of Phenol Barbital

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 C 12 H 12 N 2 O 3 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. 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.

4. Raw Materials: Benyl Cyanide , Ethanol , Diethyl carbonate , Sulfuric acid, Ethyl bromide, Urea Chemical reaction:- It is Prepared from benyl cyanide by following steps:

5. Flowchart for phenol barbital production

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.

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