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

HRID 131491
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HRID 131491 반응식
[CH:1]([C:4]1[S:13][C:12]2[NH:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[NH:8][C:7](=S)[C:6]=2[N:5]=1)([CH3:3])[CH3:2].O(C)S(C(F)(F)F)(=O)=O.[CH3:28][O:29][CH2:30][CH2:31][CH2:32][C@H:33]1[CH2:38][NH:37][CH2:36][CH2:35][NH:34]1.N1C=CC=CC=1>ClCCl>[CH3:28][O:29][CH2:30][CH2:31][CH2:32][C@@H:33]1[NH:34][CH2:35][CH2:36][N:37]([C:7]2[C:6]3[N:5]=[C:4]([CH:1]([CH3:3])[CH3:2])[S:13][C:12]=3[NH:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[N:8]=2)[CH2:38]1
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참가 물질

6

반응물 4

HCID 1049PyridineHCID 9526Methyl triflateHCID 210934792-Isopropyl-4,9-dihydro-3-thia-1,4,9-triazabenzo[f]azulene-10-thioneHCID 45099475(2S)-2-(3-Methoxypropyl)piperazine

생성물 1

HCID 135457471(S)-10-[3-(3-Methoxy-propyl)-piperazin-1-yl]-2-isopropyl-4H-3-thia-1,4,9-triaza-benzo[f]azulene

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

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).

후처리

  1. customEvaporate the mixture uner reduced pressure
  2. temperaturereflux for 8 hours
  3. concentrationConcentrate the reaction mixture under reduced pressure
  4. additiondilute the residue with ethyl acetata
  5. washWash the organic with brine twice
  6. dry with materialdry over sodium sulfate
  7. filtrationfilter
  8. concentrationconcentrate under reduced pressure
  9. customto give a residue
  10. customPurify the residue by flash chromatography
  11. washeluting with 2M ammonia in methanol:dichloromethane (5:95)

출처 및 근거

ORD 기록
ord-683ab29264ea40749610aef2cfc523d7
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07384934B2

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