反应详情

To a solution of 100 mg, 0.219 mmol) of (E)-5-(3,4-dichlorostyryl)-2,3-dihydro-1-methyl-1H-1,4-benzodiazepin-7-amine hydrochloride in 3 ml of dichloromethane was added 0.073 ml, 0.9 mmol) of pyridine, and 0.018 ml, (0.231 mmol) of methanesulphonyl chloride. The solution was stirred for 1 hour, concentrated under reduced pressure and the residue partitioned between brine and dichloromethane. The organic phase was dried over magnesium sulphate, filtered and evaporated, The residue was chromatographed on silica gel using first dichloromethane/methanol (98:2) and then dichloromethane/methanol (97:3) for the elution. There was obtained (E)-5-(3,4-dichlorostyryl)-2,3-dihydro-1-methyl-1H-1,4-benzodiazepin-7-acetamide hydrochloride as a brown solid MS: m/e 424.1 [M+H]+.

1. concentrationconcentrated under reduced pressure
2. customthe residue partitioned between brine and dichloromethane
3. dry with materialThe organic phase was dried over magnesium sulphate
4. filtrationfiltered
5. customevaporated
6. customThe residue was chromatographed on silica gel using first dichloromethane/methanol (98:2)
7. washdichloromethane/methanol (97:3) for the elution