HRID603913

反应详情

EQUATION

反应方程式

HRID 603913 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 2-mercaptoacetate (9.68 mL, 88.3 mmol) was added dropwise to a suspension of K2CO3 (12.2 g, 88.3 mmol) and 1-(1,3-benzodioxol-5-yl)-2-bromoethanone (21.4 g, 88.3 mmol) in dry acetone (100 mL). The mixture was stirred at reflux for seven hours, cooled at an icebath and added 200 mL water. Diethyl ether (400 mL) was added and the phases were separated. The aqueous layer was extracted with diethyl ether (200 mL) and the combined organic layers were washed with brine (200 mL), dried (MgSO4) and concentrated. This afforded the title compound.

WORKUP

后处理

  1. temperatureat reflux for seven hours
  2. temperaturecooled at an icebath
  3. customthe phases were separated
  4. extractionThe aqueous layer was extracted with diethyl ether (200 mL)
  5. washthe combined organic layers were washed with brine (200 mL)
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated