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Phosphorus oxychloride → 2-Chloro-1-propyl-8-[6-(3-trifluoromethyl-benzylamino)-pyridin-3-yl]-1,7-dihydro-purin-6-one

HRID 925559
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HRID 925559 반응식
[CH2:1]([N:4]1[C:12](=[O:13])[C:11]2[NH:10][C:9]([C:14]3[CH:15]=[N:16][C:17]([NH:20][CH2:21][C:22]4[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=4)=[CH:18][CH:19]=3)=[N:8][C:7]=2[NH:6][C:5]1=O)[CH2:2][CH3:3].O=P(Cl)(Cl)[Cl:35].[NH4+].[Cl-]>>[Cl:35][C:5]1[N:4]([CH2:1][CH2:2][CH3:3])[C:12](=[O:13])[C:11]2[NH:10][C:9]([C:14]3[CH:15]=[N:16][C:17]([NH:20][CH2:21][C:22]4[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=4)=[CH:18][CH:19]=3)=[N:8][C:7]=2[N:6]=1
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참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 25517Ammonium ChlorideHCID 674976141-Propyl-8-[6-(3-trifluoromethyl-benzylamino)-pyridin-3-yl]-3,7-dihydro-purine-2,6-dione

생성물 1

HCID 674981072-Chloro-1-propyl-8-[6-(3-trifluoromethyl-benzylamino)-pyridin-3-yl]-1,7-dihydro-purin-6-one수율 26%

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온도
127.5 °C

실험 절차

A mixture of 1-Propyl-8-[6-(3-trifluoromethyl-benzylamino)-pyridin-3-yl]-3,7-dihydro-purine-2,6-dione (0.2 g, 0.45 mmol), POCl3 (5 ml) and NH4Cl (0.486 g, 9 mmol) were heated at 125-130° C. for 20 hours. Reaction mixture was cooled to 20-25° C. It was then concentrated under vacuum. The residue was dissolved in water (50 ml) and precipitated solid was filtered off. The solid obtained was further purified by column chromatography to obtain pure 2-Chloro-1-propyl-8-[6-(3-trifluoromethyl-benzylamino)-pyridin-3-yl]-1,7-dihydro-purin-6-one as pale yellow solid (0.054 g, 26%).

후처리

  1. customReaction mixture
  2. temperaturewas cooled to 20-25° C
  3. concentrationIt was then concentrated under vacuum
  4. dissolutionThe residue was dissolved in water (50 ml)
  5. customprecipitated solid
  6. filtrationwas filtered off
  7. customThe solid obtained
  8. customwas further purified by column chromatography

출처 및 근거

ORD 기록
ord-16774ad2272145438553496305f1ba1f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09284316B2

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