申请人:CROMPTON & KNOWLES CORPORATION
公开号:EP0385014A1
公开(公告)日:1990-09-05
A process is disclosed for the preparation of N-substituted aminomethylphosphonic acids, particularly methylaminomethylphosphonic acid, in high yield and purity with related low production cost using conventional equipment, which comprises the steps of (a) reacting an N-substituted amide with paraformaldehyde in a low molecular weight carboxylic acid to form the N-methylol derivative, (b) reacting the N-methylolamide with PCl₃ in excess low molecular weight carboxylic acid and heating to form the phosphonomethyl derivative, (c) hydrolyzing acid chloride and acid anhydride with water, (d) distilling off the low-molecular weight carboxylic acid, (e) hydrolyzing the N-acyl group with water and strong acid catalyst, (f) adding low molecular weight alcohol to crystalline the N-substituted-aminomethyl- phosphonic acid and (g) filtering, and washing the product.
揭示了一种用于制备N-取代氨基甲基膦酸的过程,特别是高产率和纯度的甲基氨基甲基膦酸,采用常规设备相关低生产成本,包括以下步骤:(a) 在低分子量羧酸中将N-取代酰胺与多聚甲醛反应,形成N-甲基醇衍生物,(b) 将N-甲基醇酰胺与过量的三氯化膦在低分子量羧酸中反应并加热,形成膦甲基衍生物,(c) 用水水解酸氯和酸酐,(d) 蒸馏掉低分子量羧酸,(e) 用水和强酸催化剂水解N-酰基团,(f) 添加低分子量醇结晶N-取代氨基甲基膦酸,(g) 过滤并清洗产物。