格氏法制备甲基亚磷酸二乙酯工艺研究
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摘要
甲基亚磷酸二乙酯是重要的有机化工中间体,广泛应用于农药、医药等行业。为了降低其生产成本,设计了以三氯化磷为起始原料,经歧化反应合成中间体氯代亚磷酸二乙酯,再与自制的格氏试剂甲基氯化镁反应合成甲基亚磷酸二乙酯。实验考查并优化了原料配比、反应温度、保温时间等一系列条件,所得甲基亚磷酸二乙酯的总收率可达87%,纯度达98.5%。
Diethyl methylphosphonite is a key intermediate in organic chemical industry,widely used in pesticides,pharmaceuticals and other industries. In order to diminish the cost of production of its relevant products, we determine using phosphorus trichloride and triethyl phosphite to give diethyl phosphonate chloride, and then with the homemade Grignard reagent methyl magnesium chloride reaction of diethyl methyl phosphite. The conditions such as the ratio of raw materials,reaction temperature, solvent dosage and holding time were investigated and optimized. The total yield of diethyl methylphosphonite was up to 87% or more, the purity of up to 98.5%.
Diethyl methylphosphonite is a key intermediate in organic chemical industry,widely used in pesticides,pharmaceuticals and other industries. In order to diminish the cost of production of its relevant products, we determine using phosphorus trichloride and triethyl phosphite to give diethyl phosphonate chloride, and then with the homemade Grignard reagent methyl magnesium chloride reaction of diethyl methyl phosphite. The conditions such as the ratio of raw materials,reaction temperature, solvent dosage and holding time were investigated and optimized. The total yield of diethyl methylphosphonite was up to 87% or more, the purity of up to 98.5%.
引文
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[6] MICHALSKI J. Preparation of diethyl phosphonite chloride[J].Journal of the Chemical Society,1961(4):904.
[2]丁成荣,吕兆斌,李伟华,等.2-氨基甲基-3-氯-5-三氟甲基吡啶盐酸盐的合成[J].浙江工业大学学报,2014,42(4):435-439.
[3]蒋红英,刘书来,张建友,等.有机磷和菊酯类农药在蔬菜中的氧化消降技术研究[J].浙江工业大学学报, 2010, 38(4):368-371.
[4]联邦德国Hoechst公司农业开发部.草丁膦[J].农药译丛,1985,7(1):62-64.
[5] MILFS J A. Improved reproducible procedures for the preparation of diethyl methyl phosphonite[J].Organic Preparations and Procedures International, 1979,11(1):11-16.
[6] MICHALSKI J. Preparation of diethyl phosphonite chloride[J].Journal of the Chemical Society,1961(4):904.