HRID22165

反应详情

EQUATION

反应方程式

HRID 22165 的结构方程式

PROCEDURE

实验过程

1.0 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) is introduced into a solution of 2.1 g of potassium cyanide in 15 ml of water and the whole is treated dropwise at from -7° to -3° C., with cooling, over a period of 10 minutes, with 10 ml of concentrated hydrochloric acid. It is subsequently stirred at room temperature for approximately 16 hours and the crystals which have separated are then filtered off. They are washed with water and recrystallised from acetone/n-hexane to yield 0.2 g of 3-carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see also Example 17).

WORKUP

后处理

  1. additionthe whole is treated dropwise at from -7° to -3° C.
  2. customthe crystals which have separated
  3. filtrationare then filtered off
  4. washThey are washed with water
  5. customrecrystallised from acetone/n-hexane