HRID574235

反应详情

EQUATION

反应方程式

HRID 574235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A cooled (0° C.) solution of benzyl 3,3,3-trifluoro-2-hydroxy-2-methylpropanoate (Int. D1) (100 mg, 0.403 mmol) in DMF (4 ml) was treated with sodium hydride (16.11 mg, 0.403 mmol) followed by benzyl bromide (0.048 ml, 0.403 mmol) and stirred at 0° C. for 2 h. The reaction mixture was allowed to warm to room temperature and stirring continued for a further 3 hrs. The reaction mixture was partitioned between EtOAc and 0.1M HCl solution. The organic phase was washed with saturated brine, dried over magnesium sulfate and concentrated in vacuo to afford the title compound as an oil.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. stirringstirring
  3. waitcontinued for a further 3 hrs
  4. customThe reaction mixture was partitioned between EtOAc and 0.1M HCl solution
  5. washThe organic phase was washed with saturated brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated in vacuo