N-(5-chloropyridin-2-yl)-2-nitrobenzamide → 2-amino-N-(5-chloropyridin-2-yl)benzamide

HRID 988593

反応式

HRID 988593 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=[O:19])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[N+:16]([O-])=O)=[N:6][CH:7]=1>C1COCC1.C(OCC)(=O)C.[Ni]>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=[O:19])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[NH2:16])=[N:6][CH:7]=1

参加物

5

反応物 1

HCID 766647N-(5-chloropyridin-2-yl)-2-nitrobenzamide

生成物 1

HCID 219063812-amino-N-(5-chloropyridin-2-yl)benzamide収率 84.1%

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of N-(5-chloropyridin-2-yl)-2-nitrobenzamide (2 g, 7.2 mmol) in THF (50 mL) and ethyl acetate (50 mL) was added Raney Ni (0.2 g) and the mixture was placed under hydrogen (4.1 bar) in a high pressure apparatus. After shaking overnight, the mixture was filtered and concentrated in vacuo and purified by flash chromatography to give 1.5 g (83%) of an off-white solid.

後処理

  1. filtrationthe mixture was filtered
  2. concentrationconcentrated in vacuo
  3. custompurified by flash chromatography

出典と根拠

ORDレコード
ord-6020b4129ac14af9b3142e11d97f1ee8
出典データセット
uspto-grants-2003_10
特許番号
US06635657B1

関連ノート

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