HRID1873830

反应详情

EQUATION

反应方程式

HRID 1873830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a 250 ml round bottom flask was added tert-butyl 4-{1-[(methylsulfonyl)oxy]ethyl}piperidine-1-carboxylate (11 g, 35.8 mmol), 3-(trifluoromethyl)benzenethiol (7.6 g, 43 mmol), K2CO3 (9.9 g, 72 mmol) and 80 ml dimethylformamide. The reaction mixture was heated at 50° C. for 36 hr under N2, then cooled down to room temperature, 150 ml ether was added. The resulting mixture was sequentially washed with 250 ml water, 100 ml 5% KOH solution and 75 ml brine. The organic layers were dried over sodium sulfate, filtered and concentrated to give 13.7 g crude product. It was used for next step without further purification.

WORKUP

后处理

  1. temperaturecooled down to room temperature
  2. washThe resulting mixture was sequentially washed with 250 ml water, 100 ml 5% KOH solution and 75 ml brine
  3. dry with materialThe organic layers were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated