HRID1660737

反应详情

EQUATION

反应方程式

HRID 1660737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

To a mixture of methyl-5-thiazol-2-yl-1H-[1,2,4]triazole (6.55 g; 39 4 mmol) and dimethylformamide (32 mL), add N-bromosuccinimide (14 g, 78.8 mmol) in three portions over 1 h. Stir the mixture at 22° C. for 18 h and then add to water (300 mL) chilled to 0-5° C. Separate the aqueous layer and extract with methyl-t-butyl ether (2×200 mL). Combine the organic layers and wash with 7% aqueous sodium hydrogen carbonate (100 mL) and then dry over sodium sulfate. Filter and evaporate the solvent to afford the title compound (9.5 g, 93%). ES/MS m/z (79Br/81Br) 245/247 (M+1)+.

WORKUP

后处理

  1. temperaturechilled to 0-5° C
  2. customSeparate the aqueous layer
  3. extractionextract with methyl-t-butyl ether (2×200 mL)
  4. washCombine the organic layers and wash with 7% aqueous sodium hydrogen carbonate (100 mL)
  5. dry with materialdry over sodium sulfate
  6. filtrationFilter
  7. customevaporate the solvent