HRID1270340

反应详情

EQUATION

反应方程式

HRID 1270340 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

Sodium nitrite (0.91 g, 13.3 mmol) was added to an ice-cooled solution of 3,5-difluoro-4-morpholin-4-yl-phenylamine (0.95 g, 4.4 mmol), obtained in Preparation 6, in 6N HCl (30 mL) and the resulting yellow solution was stirred at 0° C. for 2 h. To this mixture was added an aqueous solution containing sodium azide (0.575 g, 8.86 mmol) and sodium acetate (57.5 g, 88.6 mmol). The reaction mixture was then extracted with ethyl acetate (50 mL×2) and the combined extracts were washed with 5% sodium bicarbonate solution followed by brine and dried over sodium sulfate. Evaporation of volatiles yielded the title compound as brown solid (1 g, 96%).

WORKUP

后处理

  1. additionTo this mixture was added an aqueous solution
  2. extractionThe reaction mixture was then extracted with ethyl acetate (50 mL×2)
  3. washthe combined extracts were washed with 5% sodium bicarbonate solution
  4. dry with materialdried over sodium sulfate
  5. customEvaporation of volatiles