Water → N-[(1-butylpyrrolidin-2-yl)methyl]-2-methyl-5-sulfamoyl-2,3-dihydro-1-benzofuran-7-carboxamide

Participants

Reaction Steps

A suspension of 4.4 g methyl 2-methyl-5-sulfamoyl-2,3-dihydrobenzofuran-7-carboxylate and 3.3 g of 1-butyl-2-aminomethylpyrrolidine in 25 ml of diethylene glycol is heated at 120°-130° C. and stirred for 18-20 hours. The reaction solution is cooled to room temperature and added slowly to 150 ml-200 ml of water while stirring. Under ice-cooling crystals are precipitated thoroughly and collected by suction filtration. The crude crystals are dried and recrystallized from ethyl acetate to give crystals of N-(1-butyl-2-pyrrolidinylmethyl)-2-methyl-5-sulfamoyl-2,3-dihydrobenzofuran-7-carboxamide, m.p. 169.5°-170.5° C.

Provenance & Evidence