HRID605852

反应详情

EQUATION

反应方程式

HRID 605852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 250 ml round bottom flask containing 2.2 g (8.49 mmol) of 2,2,2-trifluoro-N-((1R,4R)-4-hydroxy-1,2,3,4-tetrahydronaphthalen-1-yl)acetamide and 1.73 g (25.48 mmol) of imidazole was added 35 ml of DMF, and stirring was started. To this solution was added 4.67 g (16.99 mmol) of t-butylchlorodiphenylsilane. The reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with 150 ml EtOAc, and washed with 20 ml distilled water. The organic phase was dried over MgSO4 and concentrated in vacuo and purified by column chromatography (eluting with 1:1 DCM:Hex), to give 4.0 g (95%) of the titled compound.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at room temperature overnight
  2. washwashed with 20 ml
  3. distillationdistilled water
  4. dry with materialThe organic phase was dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. custompurified by column chromatography (eluting with 1:1 DCM:Hex)