HRID1934514

反应详情

EQUATION

反应方程式

HRID 1934514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 15 g (0.134 mol) of 2-methyl-1-cyclohexanone (7) and 23.84 g (0.134 mol) of N-bromosuccinimide in 150 mL of carbon tetrachloride was stirred and heated to reflux for 12 h under argon. The mixture was cooled to room temperature, filtered through Celite to remove succinimide and the filter cake was washed with 150 mL of ether. The filtrate was concentrated to give 25.6 g (100% yield) of 2-bromo-2-methyl-1-cyclohexanone. 1H NMR δ3.21 (td, J=16 Hz, 8 Hz, 1H, CH—CO), 2.36 (m, 2H), 2.06 (m, 2H), 1.82 (s, 3H, Me), 1.77 (m, 2H), 1.62 (m, 1H).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 12 h under argon
  3. filtrationfiltered through Celite
  4. customto remove succinimide
  5. washthe filter cake was washed with 150 mL of ether
  6. concentrationThe filtrate was concentrated