Dimethyl Sulfoxide → HCID 10279968, compound

Participants

Reaction Steps

The title compound was prepared according to the procedure of Example 6, Step D, from pyridin-3-yl-methylamine (0.515 mL, 5.057 mmol), 2,2,2-trichloro-1-{10-[(2′-methoxy-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone (1.30 g, 2.41 mmol), triethylamine (0.738 mL, 5.30 mmol), dimethylsulfoxide (0.854 mL, 12.04 mmol) and acetonitrile (15 mL). The crude material was purified by flash column chromatography on silica gel Merck-60 using 4% methanol in dichloromethane as the eluant to give a light yellow solid. The solid was taken up in dichloromethane and precipitated by the addition of diethyl ether and ethyl acetate. The precipitate was collected by filtration and dried under reduced pressure to give the title compound (0.69 g, 54%) of as a white solid, m.p. 123-127° C.

Provenance & Evidence