HRID1241873

反应详情

EQUATION

反应方程式

HRID 1241873 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

10 g (0.0734 mol) of 2-methylphenethyl alcohol were dissolved in 200 mL of dry CH2Cl2 under a nitrogen atmosphere; the solution was cooled to 5° C., 16.4 mL (0.1175 mol) of triethylamine were added, followed by a solution of 9.1 mL (0.1175 mol) of methanesulphonyl chloride in 100 mL of dry CH2Cl2, keeping the temperature below 15° C. The reaction mixture was allowed to warm to room temperate in 2 h, then 250 mL of water were added, the organic phase was collected and the solvent was removed in vacuo. The resulting oil was taken up in Et2O, the organic phase was washed with 1N HCl and with saturated NaHCO3 solution, then it was dried and the solvent was removed in vacuo, yielding 14.5 g of the title product which was used without further purification.

WORKUP

后处理

  1. customthe temperature below 15° C
  2. temperatureto warm to room temperate in 2 h
  3. customthe organic phase was collected
  4. customthe solvent was removed in vacuo
  5. washthe organic phase was washed with 1N HCl and with saturated NaHCO3 solution
  6. customit was dried
  7. customthe solvent was removed in vacuo