反应详情

温度

200 °C

Add 2-trifluoromethyl-5H-dibenzo[b,e][1,4]diazepine-11-ylamine (0.438 g, 1.58 mmol), (S)-2-(3-methoxy-propyl)-piperazine (0.25 g, 1.58 mmol) in NMP (2.8 mL). Heat at 200° C. with stirring. After 2 hours, stop heating and allow the reaction mixture cool down to ambient temperature. Add brine and extract with ethyl acetate. Wash the organic solution with brine three times, 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):419.05 (M+1).

1. temperaturestop heating
2. temperaturecool down to ambient temperature
3. extractionAdd brine and extract with ethyl acetate
4. washWash the organic solution with brine three times
5. dry with materialdry over sodium sulfate
6. filtrationfilter
7. concentrationconcentrate under reduced pressure
8. customto give crude residue
9. customPurify the residue by flash chromatography
10. washeluting with 2M ammonia in methanol:dichloromethane (5:95)