Chen Zhao
2000
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Journal
Fine chemicals
Abstract
The synthetic conditions of 4,4 dimethyl 3 oxopentanenitrile prepared sequentially from acetone through pinacol,pinacolone and α chloropinacolone were investigated.For the halogenation reaction of pinacolone,the yield of chlorination was higher than that of bromination.The yield of reaction of chloropinacolone with sodium cyanide was higher than that of bromopinacolone.The chlorination was carried out in solvent,anhydrous methanol,at 0~15 ℃.The mass ratio of solvent to pinacolone was 2.5∶1.0.The amount of chlorine gas as chlorination agent shouldn't exceed the calculated amount.The flow rate of chlorine gas should be appropriate so as to prevent the temperature of the reaction mixture going up excessively and to avoid the formation of dichloride.The solvent methanol was distilled under vacuum after reaction and used again in next batch of chlorination.For synthesis of 4,4 dimethyl 3 oxopentanenitrile,an aqueous solution of sodium cyanide was added gradually into the solution of chloropinacolone in methanol and the reaction mixture was acidified under cooling.