反应详情

Under ice-salt cooling, 4.90 g (122 mmol) of sodium hydroxide was dissolved in 50 ml of water, to which 1.6 ml (31.0 mmol) of bromine was added dropwise. This mixture was added to a solution of 100 ml of 90% dioxane containing 2.85 g (7.50 mmol) of 5-acetyl-2-[(4-chlorophenyl)sulfonylaminomethyl]indan under cooling in an ice-salt bath. Thereafter, stirring was conducted for 1 hour during which the temperature of the mixture was elevated to room temperature. The reaction solution was added with 10% sodium thiosulfate, and made acidic with 1N HCl, followed by extracting with ethyl acetate. The solvent was removed, and the residue was recrystallized from acetic acid to obtain 2.36 g of colorless crystals. Yield: 86%

1. additionwas added dropwise
2. temperatureunder cooling in an ice-salt bath
3. customwas elevated to room temperature
4. extractionby extracting with ethyl acetate
5. customThe solvent was removed
6. customthe residue was recrystallized from acetic acid