HRID1771020

反应详情

EQUATION

反应方程式

HRID 1771020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product of Example 32 (2.6 g, 9 mmol) was dissolved in dichloromethane, and the mixture was cooled in an ice-water bath, then 48% hydrobromic acid (0.54 mL, 10 mmol) was added dropwise, after the addition was complete, it was reacted at room temperature for 16 hours. After that, water was added therein for separating, the aqueous phase was extracted with dichloromethane three times, then the organic phases were combined, washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated to give the target compound 2.7 g, yield: 87%.

WORKUP

后处理

  1. temperaturethe mixture was cooled in an ice-water bath
  2. additionafter the addition
  3. customit was reacted at room temperature for 16 hours
  4. customfor separating
  5. extractionthe aqueous phase was extracted with dichloromethane three times
  6. washwashed with saturated brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated