反应详情

A mixture of 3 g (7.1 mmole) of 7-chloro-5-(2-fluorophenyl)-2,3-dihydro-N-hydroxy-α-(4-morpholinyl)-1H-1,4-benzodiazepine-2-methanimine 4-oxide, 0.6 g (20 mmole) of paraformaldehyde, 100 ml of ethanol and 250 mg of paratoluene sulfonic acid hydrate was heated to reflux for 16 hours. The crude product obtained after the usual workup was chromatographed over 60 g of silica gel using 5% (v/v) of ethanol in methylene chloride for elution. The clean fractions of product were combined and evaporated. The residue was crystallized from ether and recrystallized from ethyl acetate/hexane for analysis to yield end product as yellow crystals with mp 200°-203° C.

1. temperaturewas heated
2. temperatureto reflux for 16 hours
3. customThe crude product obtained after the usual workup
4. customwas chromatographed over 60 g of silica gel using 5% (v/v) of ethanol in methylene chloride for elution
5. customevaporated
6. customThe residue was crystallized from ether
7. customrecrystallized from ethyl acetate/hexane for analysis
8. customto yield end product as yellow crystals with mp 200°-203° C.