反応 #218673

反応方程式

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

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他Evaporate the mixture uner reduced pressure
2. 2
   温度reflux for 8 hours
3. 3
   濃縮Concentrate the reaction mixture under reduced pressure
4. 4
   workup.ADDITIONdilute the residue with ethyl acetata
5. 5
   洗浄Wash the organic with brine twice
6. 6
   乾燥dry over sodium sulfate
7. 7
   ろ過filter
8. 8
   濃縮concentrate under reduced pressure
9. 9
   その他to give a residue
10. 10
    その他Purify the residue by flash chromatography
11. 11
    洗浄eluting with 2M ammonia in methanol:dichloromethane (5:95)

実験手順

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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