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4-Methylmorpholine → N-(4-fluoro-benzyl)-4-(3-phenyl-indole-1-sulfonyl)-benzamide

HRID 737046
ノート
印刷プレビュー

反応式

HRID 737046 の反応式
[C:1]1([C:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:9]([S:16]([C:19]3[CH:27]=[CH:26][C:22]([C:23](O)=[O:24])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CN1CCOCC1.[F:35][C:36]1[CH:43]=[CH:42][C:39]([CH2:40][NH2:41])=[CH:38][CH:37]=1>C1COCC1>[F:35][C:36]1[CH:43]=[CH:42][C:39]([CH2:40][NH:41][C:23](=[O:24])[C:22]2[CH:26]=[CH:27][C:19]([S:16]([N:9]3[C:10]4[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=4)[C:7]([C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)=[CH:8]3)(=[O:17])=[O:18])=[CH:20][CH:21]=2)=[CH:38][CH:37]=1
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 79724-MethylmorpholineHCID 673264-FluorobenzylamineHCID 589751414-(3-Phenyl-indole-1-sulfonyl)-benzoic acid

生成物 1

HCID 11465854N-(4-fluoro-benzyl)-4-(3-phenyl-indole-1-sulfonyl)-benzamide収率 75.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

In a 100 ml RBF combine 4-(3-phenyl-indole-1-sulfonyl)-benzoic acid (2.5 g, 6.62 mmol) and THF (25 ml). Cool the solution in an ice water bath and add 4-methylmorpholine (0.73 ml, 7.29 mmol) follow by the portion wise addition of CDMT (1.16 g, 7.29 mmol). Stir the solution in an ice water bath for one hour. Add dropwise, a solution of 4-fluorobenzylamine (0.83 ml, 7.29 mmol) in THF (8 μl) to the reaction at 0° C. Stir the solution at 0° C. for five hours, and quench with 1N HCl (50 ml). Extract the reaction MTBE (2×50 ml), filter and wash with saturated aqueous sodium chloride (50 ml). Dry the organics over magnesium sulfate, filter and concentrate to give N-(4-fluoro-benzyl)-4-(3-phenyl-indole-1-sulfonyl)-benzamide (2.43 g) as a white solid. HPLC=95.5%, MS (ESI) m/z observed 485.1334 calculated 485.1335 (M+H).

後処理

  1. temperatureCool the solution in an ice water bath
  2. additionfollow by the portion wise addition of CDMT (1.16 g, 7.29 mmol)
  3. additionAdd dropwise
  4. stirringStir the solution at 0° C. for five hours
  5. customquench with 1N HCl (50 ml)
  6. extractionExtract
  7. customthe reaction MTBE (2×50 ml)
  8. filtrationfilter
  9. washwash with saturated aqueous sodium chloride (50 ml)
  10. dry with materialDry the organics over magnesium sulfate
  11. filtrationfilter
  12. concentrationconcentrate

出典と根拠

ORDレコード
ord-2d5d9852f2cc4ba6b1a065c6c4cd6ec2
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07595339B2

反応ノート

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