Реакция #218673

Уравнение реакции

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

Растворители

dichloromethane

Условия реакции

Обработка

1. 1
   ДругоеEvaporate the mixture uner reduced pressure
2. 2
   Температураreflux for 8 hours
3. 3
   КонцентрированиеConcentrate the reaction mixture under reduced pressure
4. 4
   workup.ADDITIONdilute the residue with ethyl acetata
5. 5
   ПромывкаWash the organic with brine twice
6. 6
   Сушкаdry over sodium sulfate
7. 7
   Фильтрацияfilter
8. 8
   Концентрированиеconcentrate under reduced pressure
9. 9
   Другоеto give a residue
10. 10
    ДругоеPurify the residue by flash chromatography
11. 11
    Промывкаeluting with 2M ammonia in methanol:dichloromethane (5:95)

Методика

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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