反应详情

Add (S)-2-trifluoromethyl-11-[3-(3-methoxy-propyl)-piperazin-1-yl]-5H-dibenzo[b,e][1,4]diazepine (0.167 g, 0.399 mmol), formaldehyde (40.8 mg, 0.499 mmol, 37%), and sodium triacetoxyborohydride (0.127 g, 0.598 mmol) in dichloromethane (3 mL). Stir at ambient temperature over night. Dilute the mixture with water and extract with dichloromethane. Wash the organic with brine twice, dry over sodium sulfate, filter, and concentrate under reduced pressure to give crude residue. Purify the residue by flash chromatography, eluting with 2M ammonia in methanol:dichloromethane (5:95) to give the title compound: mass spectrum (m/e):433.08 (M+1).

1. extractionextract with dichloromethane
2. washWash the organic with brine twice
3. dry with materialdry over sodium sulfate
4. filtrationfilter
5. concentrationconcentrate under reduced pressure
6. customto give crude residue
7. customPurify the residue by flash chromatography
8. washeluting with 2M ammonia in methanol:dichloromethane (5:95)