HRID1869322

反应详情

EQUATION

反应方程式

HRID 1869322 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.47 g (8.46 mmol) of 2-(bromomethyl)-5-fluoro-3-nitrobenzoic acid methyl ester is mixed with 8.3 ml of N,N-dimethylformamide and 5.5 ml of water. After 0.82 g (12.66 mmol) of sodium azide is added, the batch is stirred overnight. The reaction mixture is added to water and extracted three times with methyl tert-butyl ether. The combined organic extracts are washed with water and with brine. After drying on sodium sulfate, it is filtered, and the solvent is spun off. Chromatography on a Flashmaster yields 2.06 g (95.8%) of the desired azide.

WORKUP

后处理

  1. extractionextracted three times with methyl tert-butyl ether
  2. washThe combined organic extracts are washed with water and with brine
  3. customAfter drying on sodium sulfate, it
  4. filtrationis filtered