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N-[(R)-Cyclopropyl(4-nitrophenyl)oxidosulphanylidene]-2,2,2-trifluoroacetamide → N-[(R)-(4-Aminophenyl)(cyclopropyl)oxidosulphanylidene]-2,2,2-trifluoroacetamide

HRID 1027845
ノート
印刷プレビュー

反応式

HRID 1027845 の反応式
[CH:1]1([S:4]([C:13]2[CH:18]=[CH:17][C:16]([N+:19]([O-])=O)=[CH:15][CH:14]=2)(=[N:6][C:7](=[O:12])[C:8]([F:11])([F:10])[F:9])=[O:5])[CH2:3][CH2:2]1>[Pd].C(O)C.C1COCC1>[NH2:19][C:16]1[CH:15]=[CH:14][C:13]([S:4]([CH:1]2[CH2:3][CH2:2]2)(=[N:6][C:7](=[O:12])[C:8]([F:11])([F:9])[F:10])=[O:5])=[CH:18][CH:17]=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 1

HCID 56949254N-[(R)-Cyclopropyl(4-nitrophenyl)oxidosulphanylidene]-2,2,2-trifluoroacetamide

生成物 1

HCID 58533486N-[(R)-(4-Aminophenyl)(cyclopropyl)oxidosulphanylidene]-2,2,2-trifluoroacetamide収率 93%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒2 回HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

1.4 g palladium on charcoal (10%/50% moisture) was added to a solution of 6.9 g (21.44 mmol) (RS)-S-cyclopropyl-S-(4-nitrophenyl)-N-(trifluoroacetyl)sulfoximide in 214 ml ethanol and 39 ml THF and was hydrogenated for 1 hour under normal pressure at 25° C. A further 1.4 g palladium on charcoal was added, and it was hydrogenated for a further 4.5 hours at normal pressure. The mixture was filtered, 1.4 g palladium on charcoal was added to the filtrate again and finally hydrogenated for 45 minutes. The mixture was filtered and concentrated by evaporation. 5.8 g (19.91 mmol; yield: 93%) of the product was obtained.

後処理

  1. waitit was hydrogenated for a further 4.5 hours at normal pressure
  2. filtrationThe mixture was filtered
  3. addition1.4 g palladium on charcoal was added to the filtrate again
  4. waitfinally hydrogenated for 45 minutes
  5. filtrationThe mixture was filtered
  6. concentrationconcentrated by evaporation
  7. custom5.8 g (19.91 mmol; yield: 93%) of the product was obtained

出典と根拠

ORDレコード
ord-dc659bd0e5c1491f95f98d8754562c31
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735412B2

反応ノート

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