HRID645593

反应详情

EQUATION

反应方程式

HRID 645593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a solution of 2-bromo-4,5-difluoro-phenol (1 g, 4.78 mmol) in N,N-dimethylformamide were added K2CO3 and 2-fluoropyridine (0.46 g, 4.78 mmol) and heated at 120° C. for overnight. One more equivalent of 2-fluoropyridine was added and heated at 150° C. for 12 h. The reaction mixture was dissolved in ethyl acetate, washed with 1M NaHCO3, concentrated and purified by flash column chromatography using 0%, 5% and 10% of ethyl acetate in hexanes to yield 0.8 g (59%) of product. MS (ESI+) m/z 286 (M+H)+.

WORKUP

后处理

  1. temperatureheated at 150° C. for 12 h
  2. washwashed with 1M NaHCO3
  3. concentrationconcentrated
  4. custompurified by flash column chromatography