反应详情

温度

-20 °C

5.33 g (40.0 mmol) of anhydrous aluminum chloride was suspended in 20 ml of methylenechloride and added with 1.61 g (5.00 mmol) of 2-[(4-chlorophenyl)sulfonylaminomethyl]indan, followed by cooling at -20° C. 10 ml of methylene chloride containing as dissolved 0.68 ml (7.5 mmol) of dichloromethylmethylether was slowly added dropwise thereto, followed by stirring for 1 hour at the same temperature. The reaction solution was poured into ice-water and stirred for 1 hour. Thereafter, the organic phase was collected, washed, dried, and the solvent was removed. The residue was purified by silica gel column chromatography (chloroform), followed by recrystallizing from a solvent mixture of ethylacetate and hexane to obtain 375 mg of colorless crystals. Yield: 22%

1. additionwas slowly added dropwise
2. stirringstirred for 1 hour
3. customThereafter, the organic phase was collected
4. washwashed
5. customdried
6. customthe solvent was removed
7. customThe residue was purified by silica gel column chromatography (chloroform)
8. customby recrystallizing from a solvent mixture of ethylacetate and hexane