HRID439672
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 (31×40 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
- temperatureThe mixture was cooled to room temperature
- extractionextracted with ether (2×75 mL)
- extractionThe ether extract
- washwas washed with water (31×40 mL), brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe residue obtained
- customafter evaporation of the solvent
- customwas chromatographed over silica gel