Reaktion #218673

Reaktionsgleichung

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

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeEvaporate the mixture uner reduced pressure
2. 2
   Temperaturreflux for 8 hours
3. 3
   EinengenConcentrate the reaction mixture under reduced pressure
4. 4
   workup.ADDITIONdilute the residue with ethyl acetata
5. 5
   WaschenWash the organic with brine twice
6. 6
   Trocknendry over sodium sulfate
7. 7
   Filtrationfilter
8. 8
   Einengenconcentrate under reduced pressure
9. 9
   Sonstigeto give a residue
10. 10
    SonstigePurify the residue by flash chromatography
11. 11
    Wascheneluting with 2M ammonia in methanol:dichloromethane (5:95)

Vorschrift

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).

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