HRID1097278

反应详情

EQUATION

反应方程式

HRID 1097278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
153 °C

PROCEDURE

实验过程

A mixture of 5-amino-1,5-dimethylbarbituric acid hydrochloride (0.42 g, 2 mmol), tetrafluorophthalic anhydride (0.44 g, 2 mmol), Et3N (0.28 mL, 0.20 g, 2 mmol) and DMSO (3 mL) was stirred and heated at 153° C. for 5 hours. The reaction mixture was then allowed to cool down to room temperature and poured into water (10 mL). The oil that immediately formed was carefully removed from the solution, from which a solid precipitated after 4 days standing at room temperature. The precipitate was collected by filtration, washed with water and dried under reduced pressure to give 20a as yellow crystals.

WORKUP

后处理

  1. temperatureto cool down to room temperature
  2. customThe oil that immediately formed
  3. customwas carefully removed from the solution, from which a solid
  4. customprecipitated after 4 days
  5. customstanding at room temperature
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water
  8. customdried under reduced pressure