正丁基硫代磷酰三胺的合成工艺改进

Improved synthesis of N-n-butylthiophosphoric triamide

摘要:

以三氯硫磷和正丁胺为原料采用管式反应器制得关键中间体正丁基硫代二磷酰氯，然后室温通氨气反应3h制得正丁基硫代磷酰三胺，总收率达65.1%。目标化合物经IR、ESI-MS、1H-NMR和13C-NMR表征确认，重点考察了原料配比、反应温度、停留时间对反应总收率的影响，优化的合成工艺参数为：投料配比n（三氯硫磷）：n（正丁胺）= 1 : 1.5，停留时间为30s，管长14m，管径3mm，反应温度28~30℃。

Abstract:

The improved procedure for preparing N-n-butylthiophosphoric triamide was described. The important intermediate N-n-butylaminothiophosphoryl dichloride was synthesized from thiophosphoryl chloride reacted with n-butylamine in the tubular reactor, followed by ammonolysis by NH3 for about 3h to give the title compound. The overall yield was 65.1%. The structure of the product was characterized by IR、ESI - MS、1H - NMR and 13C - NMR. In the meanwhile, a few factors including molar ratio of raw materials, reaction temperature and residence time are investigated. And the optimum condition were: Molar ratio of thiophosphoryl chloride to n-butylamine is 1 : 1.5, residence time is 30s, tube length 14m, tube diameter 3mm, 28 ~ 30℃。