HRID1528377

反应详情

EQUATION

反应方程式

HRID 1528377 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

To a solution of (3-(trifluoromethyl)isoxazol-5-yl)methanol (2.5 g, 15 mmol) in dimethylformamide (25 mL) was added drop wise tribromophosphine (4.64 g 17.1 mmol, 1.15 eq) and the mixture was stirred at 0° C. for 15 min and at ambient temperature for 2 h. The reaction mixture was partitioned between 10% sodium bicarbonate and dichloromethane. The phases were separated and the organic phase was washed with water and passed over a plug of silica eluting with dichloromethane. The UV active product fractions were collected and evaporated to yield the title compound as colorless oil (2.04 g 59.3%), MS 229 and 231 (M.)+.

WORKUP

后处理

  1. customThe reaction mixture was partitioned between 10% sodium bicarbonate and dichloromethane
  2. customThe phases were separated
  3. washthe organic phase was washed with water
  4. customThe UV active product fractions were collected
  5. customevaporated