HRID647793

反应详情

EQUATION

反应方程式

HRID 647793 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl N-[[[[[(5,5-dimethyl-2-thioxo-1,3,2-dioxaphosphorinan-2-yl)(methyl)amino]sulfinyl]methylamino]carbonyl]oxy]ethanimidothioate was prepared by the procedure employed in Example 9, by reacting methyl N-[[(methylamino)carbonyl]oxy]ethanimidothioate (2.43 g, 0.015 mole), thionyl chloride (1.79 g, 0.015 mole), and 5,5-dimethyl-2-methylamino-2-thioxo-1,3,2-dioxaphosphorinan (2.93 g, 0.015 mole) in pyridine (10 ml). Recrystallization from chloroform-hexane afforded 3.0 g of needles of the formula below, mp 112~114°. ##STR33##

WORKUP

后处理

  1. customRecrystallization from chloroform-hexane