HRID1835031

反应详情

EQUATION

反应方程式

HRID 1835031 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(2R)-2-(4-Chlorophenyl)-2-cyclopropylethanol (6.50 g, 33.0 mmol), tosyl chloride (7.86 g, 41.0 mmol) and 6.0 ml of triethylamine (6.0 ml) are dissolved in dichloromethane (150 ml) and allowed to stir for 3 days. The reaction mixture is washed successively with 1 N HCl (100 ml), water (100 ml) and saturated brine solution (100 ml). The organic layer is dried over anhydrous sodium sulfate and concentrated in vacuo. The residue is chromatographed on silica gel eluting with ether:hexane (10:90 to 25:75) to afford the title compound as a colorless oil (11.1 g, 96%) which is characterized by 1HNMR, 13CNMR and mass spectral analysis.

WORKUP

后处理

  1. washThe reaction mixture is washed successively with 1 N HCl (100 ml), water (100 ml) and saturated brine solution (100 ml)
  2. dry with materialThe organic layer is dried over anhydrous sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customThe residue is chromatographed on silica gel eluting with ether:hexane (10:90 to 25:75)