反应详情

The title compound was prepared by reacting 4-(2-chlorophenyl)-2-iodo-9-methyl-6H thieno[3,2-f][1,2,4]triazolo[4,3-a][1,4]diazepine with 1-(2-propynyl)-2(1H)quinolinone [ref. A. Lindquist et al., Acta Pharm. Suecica, 9,99 (1972)]as described in EXAMPLE 37. It was isolated by chromatography over 50 g of silica gel using 5% (v/v) of ethanol in methylene chloride and was further purified by rechromatography over 50 g of silica gel using tetrahydrofuran. Crystallization from ethyl acetate/methanol gave off-white crystals of 1-{3-[4-(2-chlorophenyl)-9-methyl-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a][1,4]diazepin-2-yl] 2-propynyl}-2(1H)-quinolinone with m.p. 162-165°. These crystals contained according to analytical data 0.5 molar amounts of water.

1. customwas further purified by rechromatography over 50 g of silica gel
2. customCrystallization from ethyl acetate/methanol