反应详情

温度

80 °C

A suspension of 2,2,2-trichloro-1-{10-[(2,2′,6′-trimethyl-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone of Step D (0.610 g, 1.1 mmol) and 3-(aminomethyl)pyridine (0.119 g, 1.0 mmol) in acetonitrile (15 mL), was treated with dimethylsulfoxide (0.432 g, 5.5 mmol) and triethylamine (0.246 g, 2.4 mmol). The mixture was heated under nitrogen at 80° C. overnight, and then concentrated. The residue was taken up in dichloromethane (25 mL), washed with brine and water, dried over anhydrous magnesium sulfate and concentrated. Flash chromatography of the residue on silica gel Merck-60 eluting with 85:10:5 ethylacetate:hexane:dichloromethane provided the title compound (0.275 g).

1. concentrationconcentrated
2. washwashed with brine and water
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. washeluting with 85:10:5 ethylacetate