反应详情

温度

-10 °C

20.1 g (0.1 mol) of 4-carboxy-benzenesulfonamide were suspended in 300 ml of anhydrous tetrahydrofuran, and 15.2 ml (0.11 mol) of triethylamine were added dropwise at 0° C., while stirring. After 30 minutes, 10.5 ml (0.11 mol) of ethyl chloroformate were added dropwise at 0° C., the mixture was stirred at this temperature for 1 hour and cooled to -10° C., and 12.1 g (0.1 mol, 12.5 ml) of 2-phenylethylamine in 30 ml of anhydrous tetrahydrofuran were added dropwise. After 1 hour at 0° C., the mixture was warmed to 20° C. and concentrated in vacuo and the solid residue was treated with water, filtered off with suction and recrystallized from ethanol to give 20.4 g of product, melting point 243° to 245° C.

1. stirringthe mixture was stirred at this temperature for 1 hour
2. waitAfter 1 hour at 0° C.
3. temperaturethe mixture was warmed to 20° C.
4. concentrationconcentrated in vacuo
5. additionthe solid residue was treated with water
6. filtrationfiltered off with suction
7. customrecrystallized from ethanol