反应详情

温度

22 °C

A solution of 175 g of tert-butyldimethylsilyl chloride in 100 ml of a 1:1 mixture that consists of hexane and dimethylformamide is slowly added in drops at 0° C. under nitrogen to a solution of 100 g of 2-butin-1-ol and 158 g of imidazole in 300 ml of dimethylformamide, and it is stirred for 2 hours at 0° C. and for 16 hours at 22° C. The reaction mixture is diluted with 2.5 l of ether, washed once with water, once with 5% sulfuric acid, once with water, once with saturated sodium bicarbonate solution and washed neutral with semi-saturated sodium chloride solution. After drying on sodium sulfate and filtration, it is concentrated by evaporation in a vacuum. The residue that is thus obtained is purified by chromatography on silica gel. With hexane/0–40% ether, 74.3 g of the title compound is obtained as a colorless oil.

1. washwashed once with water, once with 5% sulfuric acid, once with water, once with saturated sodium bicarbonate solution
2. washwashed neutral with semi-saturated sodium chloride solution
3. customAfter drying on sodium sulfate and filtration, it
4. concentrationis concentrated by evaporation in a vacuum
5. customThe residue that is thus obtained
6. customis purified by chromatography on silica gel