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

HRID 1291361
ノート
印刷プレビュー

反応式

HRID 1291361 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-dc3300df789c4f1f8df6632a302add1e
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05753664

反応ノート

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