HRID751571

反应详情

EQUATION

反应方程式

HRID 751571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

(1S,5R,6S)-6-(3,6-difluoro-2-methoxyphenyl)-3-oxabicyclo[3.1.0]hexan-2-one (130 mg, 0.55 mmol) was mixed with 1.2 ml of 30% HBr/AcOH (6 mmol) and heated in a sealed vessel at stirring for about 4 h at 90° C. The reaction mixture was then cooled down, mixed with water and extracted into diethyl ether (3×20 ml). Ether extract was washed with sat. sodium bicarbonate solution and brine. Dried over magnesium sulfate. Concentration gave 160 mg of white solid material. 98% yield.

WORKUP

后处理

  1. temperatureheated in a sealed vessel
  2. temperatureThe reaction mixture was then cooled down
  3. extractionextracted into diethyl ether (3×20 ml)
  4. extractionEther extract
  5. washwas washed with sat. sodium bicarbonate solution and brine
  6. dry with materialDried over magnesium sulfate
  7. concentrationConcentration