반응 #218673

반응 방정식

pyridine

2-isopropyl-4,9-dihydro-3-thia-1,4,9-triaza-benzo[f]azulene-10-thione

methyl triflate

(S)-2-(3-methoxy-propyl)-piperazine

→

title compound

(S)-10-[3-(3-Methoxy-propyl)-piperazin-1-yl]-2-isopropyl-4H-3-thia-1,4,9-triaza-benzo[f]azulene

용매

dichloromethane

반응 조건

후처리

1. 1
   기타Evaporate the mixture uner reduced pressure
2. 2
   온도reflux for 8 hours
3. 3
   농축Concentrate the reaction mixture under reduced pressure
4. 4
   workup.ADDITIONdilute the residue with ethyl acetata
5. 5
   세척Wash the organic with brine twice
6. 6
   건조dry over sodium sulfate
7. 7
   여과filter
8. 8
   농축concentrate under reduced pressure
9. 9
   기타to give a residue
10. 10
    기타Purify the residue by flash chromatography
11. 11
    세척eluting with 2M ammonia in methanol:dichloromethane (5:95)

실험 절차

Combine 2-isopropyl-4,9-dihydro-3-thia-1,4,9-triaza-benzo[f]azulene-10-thione (0.5 g, 1.816 mmol), methyl triflate (0.306 mL, 2.723 mmol) in dichloromethane (4 mL) and stir at ambient temperature for 2 hours. Evaporate the mixture uner reduced pressure and then combine the residue with (S)-2-(3-methoxy-propyl)-piperazine (0.287 g, 1.816 mmol) and pyridine (4 mL) and reflux for 8 hours. Concentrate the reaction mixture under reduced pressure and dilute the residue with ethyl acetata. Wash the organic with brine twice, dry over sodium sulfate, filter and concentrate under reduced pressure to give a 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):400.03 (M+1).

출처