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[目的]以2-(1-氯环丙基)-3-氯-1-(2-氯苯基)-2-丙醇为原料,通过肼解成盐、环合、氧化反应制得丙硫菌唑,开发丙硫菌唑合成的简便清洁工艺方法。研究肼化合物在多种溶剂中的稳定性,物料配比对环合反应的影响及丙硫菌唑合成氧化剂的筛选。[方法]经反应工艺条件优化,以乙酸乙酯为溶剂制备肼化合物盐酸盐,投料1.2 eq甲醛水溶液和1.5 eq硫氰酸钠完成环合反应,在0.1 eq三氯化铁催化下进行氧化反应。[结果]粗品经重结晶后得到灰白色固体丙硫菌唑。3步反应产品总收率56.2%,液相含量为97.5%。
[Objective] The preparation of 2- (1-chlorocyclopropyl) -3-chloro-1- (2-chlorophenyl) Thiocarbazole, the development of prothioconazole synthesis of simple and convenient cleaning process. The stability of hydrazine compounds in various solvents, the effect of the ratio of materials on the cyclization reaction and the screening of the synthetic oxidants of prothioconazole were studied. [Method] After the reaction conditions were optimized, the hydrazine hydrochloride was prepared by using ethyl acetate as the solvent. 1.2 eq formalin and 1.5 eq sodium thiocyanate were charged to complete the cyclization reaction. The reaction was catalyzed by 0.1 eq ferric chloride reaction. [Result] The crude product was obtained as an off-white solid prothioconazole after recrystallization. The total yield of 3-step reaction products was 56.2% and the liquid content was 97.5%.