HRID1199975

反应详情

EQUATION

反应方程式

HRID 1199975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred slurry of isatoic anhydride (3.10 g, 19 mmol) and S-methyl-N-(chloromethanesulfonyl)isothiourea (3.85 g, 19 mmol) in acetonitrile (30 ml) under nitrogen is added 4-(N,N-dimethylamino)pyridine (2.32 g, 19 mmol). The mixture is refluxed under nitrogen for 16 hr, concentrated, then worked up as in Example 4 above. Recrystallization from DMF provided the title compound as a white solid, mp >300° C. (1.32 g, 29%).

WORKUP

后处理

  1. temperatureThe mixture is refluxed under nitrogen for 16 hr
  2. concentrationconcentrated
  3. customRecrystallization from DMF