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Triethylamine → 2-[4-(4-Diethylphosphonooxybenzoyl)benzylthio]-3,5-dimethyl-4(3H)-quinazolinone

HRID 1291361
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인쇄 미리보기

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HRID 1291361 반응식
[OH:1][C:2]1[CH:30]=[CH:29][C:5]([C:6]([C:8]2[CH:28]=[CH:27][C:11]([CH2:12][S:13][C:14]3[N:23]([CH3:24])[C:22](=[O:25])[C:21]4[C:16](=[CH:17][CH:18]=[CH:19][C:20]=4[CH3:26])[N:15]=3)=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.[P:31](Cl)(=[O:38])([O:35][CH2:36][CH3:37])[O:32][CH2:33][CH3:34].C(N(CC)CC)C>O1CCCC1>[CH2:33]([O:32][P:31]([O:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([C:8]2[CH:28]=[CH:27][C:11]([CH2:12][S:13][C:14]3[N:23]([CH3:24])[C:22](=[O:25])[C:21]4[C:16](=[CH:17][CH:18]=[CH:19][C:20]=4[CH3:26])[N:15]=3)=[CH:10][CH:9]=2)=[O:7])=[CH:29][CH:30]=1)([O:35][CH2:36][CH3:37])=[O:38])[CH3:34]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 13139Diethyl chlorophosphateHCID 189188882-[4-(4-hydroxybenzoyl)benzylthio]-3,5-dimethyl-4(3H)-quinazolinone

생성물 1

HCID 699611962-[4-(4-Diethylphosphonooxybenzoyl)benzylthio]-3,5-dimethyl-4(3H)-quinazolinone수율 52,693.602%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2-[4-(4-hydroxybenzoyl)benzylthio]-3,5-dimethyl-4(3H)-quinazolinone (268 mg), diethyl phosphorochloridate (0.16 mg), and triethylamine (0.28 ml) were dissolved in tetrahydrofuran (8 ml) and the solution was stirred at room temperature for 14 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate. The solution was then washed with water, dried, and concentrated, and the residue was crystallized from hexane to provide the title compound as colorless solid (270 mg).

후처리

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe solution was then washed with water
  4. customdried
  5. concentrationconcentrated
  6. customthe residue was crystallized from hexane

출처 및 근거

ORD 기록
ord-dc3300df789c4f1f8df6632a302add1e
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753664

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