HRID324347

反应详情

EQUATION

反应方程式

HRID 324347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

4-(3-Chloro-4-methoxybenzyl)amino-6-cyanol-1(2H)-phthalazinone (0.20 g) prepared in Example 21 was dissolved in 5 ml of N-methyl-2-pyrrolidinone, followed by the addition of 0.14 g of t-butyl bromoacetate and 0.24 g of potassium carbonate. The obtained mixture was stirred at 80° C. for 4 hours and poured into water, followed by extraction with ethyl acetate. The organic phase was washed with water twice and with a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate and freed from the solvent by vacuum distillation. The title compound (0.41 g) was obtained as a yellow crystal.

WORKUP

后处理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic phase was washed with water twice
  3. dry with materialwith a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate
  4. distillationfreed from the solvent by vacuum distillation