反应详情

A suspension of 10 g of methyl 2-methyl-5-sulfamoyl-2,3-dihydrobenzofuran-7-carboxylate and 7.0 g of 1-ethyl-2-aminomethylpyrrolidine in 50 ml of diethylene glycol is heated at 120°-130° C. and stirred for 18 hours. The reactant solution is cooled to room temperature and added slowly with stirring to 300-400 ml of water. Under ice-cooling crystals are thoroughly deposited. The crude crystals are collected by suction filtration and washed with cold water. The crude crystals obtained are dried and recrystallized from about 220-230 ml of ethyl acetate by the use of decolorizing charcoal to give crystals of N-(1-ethyl-2-pyrrolidinylmethyl)-2-methyl-5-sulfamoyl-2,3-dihydrobenzofuran-7-carboxamide, m.p. 167°-169° C.

1. temperatureis heated at 120°-130° C.
2. additionadded slowly
3. temperatureUnder ice-cooling crystals
4. filtrationThe crude crystals are collected by suction filtration
5. washwashed with cold water
6. customThe crude crystals obtained
7. customare dried
8. customrecrystallized from about 220-230 ml of ethyl acetate by the use of decolorizing charcoal