HRID1034958

反应详情

EQUATION

反应方程式

HRID 1034958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of EXAMPLE 24C (1.78 g, 5.92 mmol) and cyclohexanone (1.23 mL, 11.85 mmol) in acetic acid (10 mL) was stirred at ambient temperature overnight and at 55° C. for 1 day. The acetic acid was removed and the residue partitioned between sodium bicarbonate solution and ethyl acetate. The organic phase was washed with water, concentrated and the residue purified by flash chromatography on silica gel using 70-90% ethyl acetate in hexane to provide the title compound as a light yellow solid (1.19 g, 53%). MS (DCI): m/z 381 (M+H)+.

WORKUP

后处理

  1. customThe acetic acid was removed
  2. customthe residue partitioned between sodium bicarbonate solution and ethyl acetate
  3. washThe organic phase was washed with water
  4. concentrationconcentrated
  5. customthe residue purified by flash chromatography on silica gel using 70-90% ethyl acetate in hexane