HRID2365441

反应详情

EQUATION

反应方程式

HRID 2365441 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 1,1-dimethylethyl 1-piperazinecarboxylate (5 g, 19.19 mmol, supplier Aldrich), in DCM (80 mL), DIPEA (5.03 mL, 28.8 mmol) was added under argon atmosphere at room temperature then 4-[(trifluoromethyl)oxy]benzenesulfonyl chloride (2.326 mL, 19.19 mmol) was added at 0° C. then ice bath was removed and the reaction mixture was stirred for 3 hrs. The reaction mixture was partitioned between DCM (30 ml) and sodium bicarbonate (2×20 ml). The organic phase was washed with HCl (2×20 ml) and water (2×20 ml), then it was dried using phase separator and DCM was removed under vacuum to give the title compound (5.5 g) as a yellow viscous liquid.

WORKUP

后处理

  1. customice bath was removed
  2. customThe reaction mixture was partitioned between DCM (30 ml) and sodium bicarbonate (2×20 ml)
  3. washThe organic phase was washed with HCl (2×20 ml) and water (2×20 ml)
  4. customit was dried
  5. customwas removed under vacuum