HRID52184

反应详情

EQUATION

反应方程式

HRID 52184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 0° C. mixture of 2-thiophenemethanol (2.80 g, 24.5 mmol) and triethylamine (5.10 mL, 36.8 mmol) in CH2Cl2 (25 mL) was added methanesulfonyl chloride (2.09 mL, 27.0 mmol) and the reaction mixture was stirred for 2 hours. The reaction mixture was poured into H2O and the layers were separated. The organic phase was washed with cold 1N HCl (3×), saturated aqueous NaHCO3, and brine, dried over MgSO4, filtered. and concentrated in vacuo. 2-thienylmethyl methanesulfonate (1.78 g, 38%) was obtained by chromatography on silica gel (20% ethyl acetate/hexane).

WORKUP

后处理

  1. customthe layers were separated
  2. washThe organic phase was washed with cold 1N HCl (3×), saturated aqueous NaHCO3, and brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationand concentrated in vacuo