反应详情

温度

0 °C

To the 250 ml 3 neck flask equipped with the thermometer, the add funnel and the stirrer, 40 ml of tetrahydrofurane or ether, 4.3 g (0.0485 mol) of N,N-dimethylaminoethylamine and 24 g (33 ml) (0.238 mol) of triethylamine or DIPEA (diisopropylethylamine) was taken up. The solution was cooled to 0° C. and the solution of 10.3 g (0.0470 mol) of sulfamoylbenzoyl chloride IX in 60 ml tetrahydrofurane or ether was added dropwise for 30 min under cooling and stirring so as the temperature did not exceed 0 to 15° C. The mixture was then stirred for 12 hours the at room temperature. 100 ml of petroleum ether or hexane was added to the mixture. The semi-solid product was filtered off and macerated with 20 ml of ice-cooled saturated aqueous sodium chloride solution. The solid product was separated, washed once with 10 ml saturated aqueous sodium chloride solution, 2 times with ice water and purified with crystallization from the water:ethanol (2:1). Afforded 6.1 g (48.0%) of 4-sulfamoyl-N-(2-dimethylaminoethyl)benzamide 1′-1. Colourless solid, m.p. 150-151° C.

1. temperatureunder cooling
2. customdid not exceed 0 to 15° C
3. stirringThe mixture was then stirred for 12 hours the at room temperature
4. filtrationThe semi-solid product was filtered off
5. temperaturecooled saturated aqueous sodium chloride solution
6. customThe solid product was separated
7. washwashed once with 10 ml saturated aqueous sodium chloride solution, 2 times with ice water
8. custompurified with crystallization from the water:ethanol (2:1)