反応 #2044443

反応方程式

1,2-propanediol

p-toluenesulfonic acid

3-chloro-2-(4-chloro-3-dimethoxymethylphenyl)-5-trifluoromethylpyridine

→

3-Chloro-2-[4-chloro-3-(4-methyl-1,3-dioxolan-2-yl)phenyl]-5-trifluoromethylpyridine

溶媒

toluene

反応条件

後処理

1. 1
   温度The mixture was then refluxed for two hours
2. 2
   抽出Extraction
3. 3
   乾燥three times with 80 ml of water each time, after which the organic solution was dried over sodium sulfate
4. 4
   濃縮concentrated
5. 5
   その他The residue was purified by chromatography on silica gel with cyclohexane/ethyl acetate (10:1)

実験手順

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);

出典