HRID1179633

反应详情

EQUATION

反应方程式

HRID 1179633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methanesulfonyl chloride (0.124 mL) was added dropwise to a stirred solution of 1-[3-(2-hydroxyethyl)phenyl]-2-pyrrolidinone (0.30 g) and triethylamine (0.42 mL) in dichloromethane (10 mL) at room temperature under an inert atmosphere. The solution was stirred for 2 hours. The reaction mixture was diluted with ethyl acetate (50 mL) and washed with water (50 mL), aqueous hydrochloric acid (1N, 2×50 mL), a saturated aqueous solution of sodium hydrogencarbonate (50 mL) and brine (50 mL). The organic layer was dried over-sodium sulfate and concentrated under reduced pressure. The crude was purified by flash chromatography on silica gel, eluting with ethyl acetate-cyclohexane (50:50) to afford the title compound in 93% yield (0.384 g).

WORKUP

后处理

  1. washwashed with water (50 mL), aqueous hydrochloric acid (1N, 2×50 mL)
  2. dry with materialThe organic layer was dried over-sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe crude was purified by flash chromatography on silica gel
  5. washeluting with ethyl acetate-cyclohexane (50:50)