反应详情

温度

23 °C

2.0 g of 1,2-propanediol and 100 mg of p-toluenesulfonic acid were added to 3.2 g of 3-chloro-2-(4-chloro-3-dimethoxymethylphenyl)-5-trifluoromethylpyridine in 100 ml of anhydrous toluene. The mixture was then refluxed for two hours and stirred at 23° C. for 16 hours. Extraction was carried out first with 50 ml of a 10% by weight sodium bicarbonate solution and then three times with 80 ml of water each time, after which the organic solution was dried over sodium sulfate and concentrated. The residue was purified by chromatography on silica gel with cyclohexane/ethyl acetate (10:1). Yield: 3.1 g (94%) of a colorless oil (1:1 mixture of diastereomers);

1. temperatureThe mixture was then refluxed for two hours
2. extractionExtraction
3. dry with materialthree times with 80 ml of water each time, after which the organic solution was dried over sodium sulfate
4. concentrationconcentrated
5. customThe residue was purified by chromatography on silica gel with cyclohexane/ethyl acetate (10:1)