HRID1732645

反应详情

EQUATION

反应方程式

HRID 1732645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

The compound of Example 1 (3.1 g), ethylene carbonate (2.0 g), and potassium hydroxide (powdered) were dissolved in dimethylformamide (50 ml) and the flask placed in an oil bath (110°-120° C.) until CO2 evolution ceased (ca. 3.5 hours). The reaction mixture was poured into water (400 ml) and chilled at 5° C. for 1 hour. The resulting precipitate was separated by filtration and recrystallized from methanol (85 ml) to obtain the title compound (68 percent yield) as pale yellow crystals, m.p. 191°-193° C.

WORKUP

后处理

  1. customthe flask placed in an oil bath
  2. custom(110°-120° C.)
  3. custom(ca. 3.5 hours)
  4. customThe resulting precipitate was separated by filtration
  5. customrecrystallized from methanol (85 ml)