HRID1948163

反应详情

EQUATION

反应方程式

HRID 1948163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.20 g (10.3 mmol) of 4-(tert-Butyl-dimethyl-silanyloxy)-1-trifluoromethyl-cyclohexanecarbaldehyde (71) were dissolved using 25 ml of anhydrous THF. 1.31 g (10.8 mmol) of 2-methyl-2-propanesulfinamide and 4.32 ml (20.6 mmol) of titanium (IV) ethoxide were added and the mixture heated for 4 h at reflux. The reaction mixture was poured into 75 ml of a saturated aqueous solution of NaHCO3 and the precipitate removed by filtration. The filtrate was extracted three times using 50 ml of ethyl acetate each. The organic layer was dried using MgSO4 and evaporated to yield 3.90 g of 72. Rt=1.02 min (Method Q).

WORKUP

后处理

  1. temperaturethe mixture heated for 4 h
  2. temperatureat reflux
  3. customthe precipitate removed by filtration
  4. extractionThe filtrate was extracted three times
  5. customThe organic layer was dried
  6. customevaporated