反应详情

In this preparation 1.0 g of sodium 1,2,4-triazole is added to a solution of 3.1 g of bis(4-fluorophenyl)methylsilylmethyl chloride in 15 mL of dimethylformamide. The mixture is heated at about 80°-90° C. for two hours and then cooled to room temperature. The mixture is then diluted with 60 ml of water and extracted three times with 50 ml portions of ethyl ether. The extracts are combined, washed twice with 80 ml of water, then with 80 ml of aqueous saturated sodium chloride solution and dried over magnesium sulfate. The ethyl ether solvent is evaporated off affording an oil which is then purified by chromatography over silica gel solution with ethyl acetate, hexane, and mixture thereof.

1. temperatureThe mixture is heated at about 80°-90° C. for two hours
2. extractionextracted three times with 50 ml portions of ethyl ether
3. washwashed twice with 80 ml of water
4. dry with materialwith 80 ml of aqueous saturated sodium chloride solution and dried over magnesium sulfate
5. customThe ethyl ether solvent is evaporated off
6. customaffording an oil which
7. customis then purified by chromatography over silica gel solution with ethyl acetate, hexane, and mixture