以邻氯苄基氯、2-氯-1-(1-氯环丙基)乙酮和水合肼等为主要原料,通过格氏反应、肼的取代、环化和氧化等4步反应合成了丙硫菌唑.目标产物及主要中间体经NMR确认,合成总收率达53%,产品质量分数为95%.该工艺具有反应条件相对温和,反应溶剂易于回收和产品质量好等特点,较适合工业化开发.
Prothioconazole was prepared successfully with 2-chlorobenzyl chloride, 2-chloro-1-(1-chlorocyclopropyl) ethanone and hydrazine hydrate, via Grignard reaction, hydrazine substitution, cyclization and oxidation. The total yield of the four synthetic steps reached 53%, and the product purity reached 95%. The procedure showed several advantages such as abundant raw materials, mild reaction conditions, easily recycled reaction solvents, easily purified intermediates and high product quality. It was suitable for industrial development.