2-甲酰肼-4-乙腈噻唑的合成
SYNTHESIS OF THE HYDRAZIDE OF 4-CYANO-METHYLTHIAZOLE-2-CARBOXYLIC ACID
-
摘要: (一)草酸硫代酰胺乙酯,在丙酮溶剂中,与1,3二氯丙酮起作用,即得2-甲酸乙酯-4-氯甲基噻唑。后者亦可用草酸酰胺乙酯,五硫化二燐和1,3二氯丙酮在甲苯中加热制得。(二)2-甲酸乙酯-4-氯甲基噻唑溶于無水甲醇与氰化鉀起反应,产生2-甲酸乙酯-4-乙腈噻唑。后者溶于乙醇,在室温情况下,与85%肼起作用,即成2-甲酰腓-4-乙腈噻唑。Abstract: Ethyl thiooxamate with 1, 3-dichloroacetone in acetone gave 2-carbethoxy-4-chloromethylthiazole (m.p. 55-56℃). The latter can also be prepared by heating ethyl oxamate, phosphorus pentasulfide and 1, 3-dichloroacetone in dry toluene. Treatment of 2-carbethoxy-4-chloromethylthiazole in methyl alcohol with potassium cyanide gave 2-carbethoxy-4-cyanomethyl thiazole (m.p. 87-88℃), which reacted with hydrazine hydrate at room temperature to form the corresponding hydrazide (m.p. 161-162℃).
下载: