HRID2394969

反应详情

EQUATION

反应方程式

HRID 2394969 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 1,4-dibromo-2-chloro-1,1,2-trifluorobutane (XVI) (7.5 g, 24.6 mmol), 1-methyl-2-pyrrolidinone (14 mL) and water (2.5 mL) was heated at 130° C. for 16 hours. The mixture was cooled to room temperature, diluted with water (80 mL) and extracted with ether (2×75 mL). The ether extract was washed with water ( 3×40 mL), brine, and dried over anhydrous magnesium sulfate. The residue obtained after evaporation of the solvent was chromatographed over silica gel to give 2.9 g (49%) of the desired alcohol as a clear oil.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionextracted with ether (2×75 mL)
  3. extractionThe ether extract
  4. washwas washed with water ( 3×40 mL), brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe residue obtained
  7. customafter evaporation of the solvent
  8. customwas chromatographed over silica gel