反应详情

温度

50 °C

65 mg of 7-[2-(6-phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-azepan-2-thione (compound A1) are suspended in 4.3 ml of methanol containing ammonia (strength: 7.0 M) and heated at 50° C. for 90 hours. Subsequently, the reaction mixture is evaporated to dryness and purified by flash chromatography on LiChroprep-NH2® (eluent gradient: dichloromethane/0-100 vol. % methanol), and lyophilized from 2.0 ml of water, 5.0 ml of dioxane to afford 29.5 mg of the title compound as an amorphous, colorless solid of m.p. 117° C. (decomp.). ESI-MS: 334.3 (MH+). TLC: Rf=0.35 (LiChroprep-NH2® HPTLC, methanol/water 10:1 parts by volume).

1. customSubsequently, the reaction mixture is evaporated to dryness
2. custompurified by flash chromatography on LiChroprep-NH2® (eluent gradient: dichloromethane/0-100 vol. % methanol)