HRID584605

反应详情

EQUATION

反应方程式

HRID 584605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A solution of N-(5-Chloro-2-hydroxy-phenyl)-acetamide (0.499 g, 2.68 mmol), K2CO3 (0.60 g, 4.35 mmol) and epibromohydrin (0.405 g, 2.95 mmol) in DMF (5 ml) was heated with stirring at 50° C. for 2 hours. The mixture was then partitioned between EtOAc and water 40+40 ml. The organic phase was washed twice with water and once with brine and finally concentrated in vacuo to give a crude product. The crude product was purified on silica (heptane:EtOAc, 1:1), to give 0.43 g (66%) of a white solid.

WORKUP

后处理

  1. customThe mixture was then partitioned between EtOAc and water 40+40 ml
  2. washThe organic phase was washed twice with water and once with brine
  3. concentrationfinally concentrated in vacuo
  4. customto give a crude product
  5. customThe crude product was purified on silica (heptane:EtOAc, 1:1)