反应详情

温度

60 °C

To a solution of 1.0 g of 4-methyl-5-hexynyl methanesulfonate and 1.1 g of (3,3,3-trifluoropropylsulfonyl)acetonitrile in 30 ml of dimethyl sulfoxide was added 0.7 g of potassium carbonate at room temperature. The reaction mixture was stirred at 60° C. for 2 days. The reaction mixture was allowed to stand to cool to nearly room temperature. To the reaction mixture was added 10% hydrochloric acid and then extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The obtained residue was subjected to silica gel chromatography to obtain 0.45 g of 6-methyl-2-(3,3,3-trifluoropropylsulfonyl)-7-octynenitrile (hereinafter referred to as the present compound (28)).

1. temperatureto cool to nearly room temperature
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with a saturated sodium chloride aqueous solution
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure