HRID1593642

反应详情

EQUATION

反应方程式

HRID 1593642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-bromobenzenethiol (2.92 g, 15.45 mmol) in 20 mL acetone was added K2CO3 (2.2 g, 15.18 mmol) and a solution of ethyl 4-bromo-3-oxocyclohexanecarboxylate (3.73 g, 15 mmol) in acetone (10 mL). The resulting suspension was stirred at room temperature for 2 hour, and then was partitioned between water and hexane. The organic layer was washed with water, then brine, then was dried over MgSO4, filtered, and concentrated. Purification by chromatography on silica gel (15% EtOAc in hexane) afforded 3.4 g (61%) of the title compound as an oil: MS (ES) m/z=356 [M]+.

WORKUP

后处理

  1. customwas partitioned between water and hexane
  2. washThe organic layer was washed with water
  3. dry with materialbrine, then was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by chromatography on silica gel (15% EtOAc in hexane)