HRID1093295

反应详情

EQUATION

反应方程式

HRID 1093295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

500 mg (3.5 mmol) 3-amino-thiophene-2-carboxamide is dissolved in 30 mL dioxane. 520 mg (1.75 mmol, 0.5 eq) triphosgene is added and the mixture is heated at 80 C for 1 h. The mixture is concentrated and triturated from hot methanol. The resulting solids are collected. The filtrate is concentrated and triturated again from hot methanol. The 2 crops of solids are combined to give 432 mg of the title compound (2.57 mmol, 73%).

WORKUP

后处理

  1. temperaturethe mixture is heated at 80 C for 1 h
  2. concentrationThe mixture is concentrated
  3. customtriturated from hot methanol
  4. customThe resulting solids are collected
  5. concentrationThe filtrate is concentrated
  6. customtriturated again from hot methanol