反应详情

1,2-Dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin6-thione (4 g) was added to a solution of dimethylaminoacetic hydrazide hydrochloride (2 g) and triethylamine (2.4 ml) in dimethylformamide (25 ml). The mixture was refluxed overnight, cooled, and concentrated under reduced pressure. The residue was purified by high performance liquid chromatography (2.5% methano/dichloromethane). The appropriate fractions were triturated with dry ether to yield 2.4 g (47.2%) of product, mp 164°-165° C.

1. temperatureThe mixture was refluxed overnight
2. temperaturecooled
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by high performance liquid chromatography (2.5% methano/dichloromethane)
5. customThe appropriate fractions were triturated with dry ether