HRID1948163
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture heated for 4 h
- temperatureat reflux
- customthe precipitate removed by filtration
- extractionThe filtrate was extracted three times
- customThe organic layer was dried
- customevaporated