HRID1944495

反应详情

EQUATION

反应方程式

HRID 1944495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 1-methyl-1H-imidazole-4-carbaldehyde (0.50 g), N-bromosuccinimide (0.89 g) and chloroform (7.0 mL) was heated at reflux for 2 hours. The mixture was cooled to 0° C., diluted with saturated aqueous sodium carbonate solution (10 mL) and extracted with dichloromethane. The combined organic extract was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with a mixture of ethyl acetate and dichloromethane (0:1 to 7:10 by volume) to afford the title compound as a white solid (0.37 g).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. extractionextracted with dichloromethane
  4. extractionThe combined organic extract
  5. dry with materialwas dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by column chromatography on silica gel
  8. washeluting with a mixture of ethyl acetate and dichloromethane (0:1 to 7:10 by volume)