5-Chloro-2-nitro-n-(2-pyridyl)benzamide → 2-Amino-5-chloro-N-2-pyridinylbenzamide

HRID 427712ノート

反応式

HRID 427712 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N+:17]([O-])=O)=[C:6]([CH:16]=1)[C:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1)=[O:8]>C1COCC1.C(OCC)(=O)C.[Ni]>[NH2:17][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:16][C:6]=1[C:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1)=[O:8]

参加物

5

反応物 1

HCID 46196505-Chloro-2-nitro-n-(2-pyridyl)benzamide

生成物 1

HCID 121506942-Amino-5-chloro-N-2-pyridinylbenzamide収率 67.3%

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 5-chloro-2-nitro-N-(2-pyridyl)benzamide (4 g, 14.4 mmol) in THF (50 mL) and ethyl acetate (50 mL) was added Raney nickel (0.5 g). The mixture was placed under an atmosphere of hydrogen (4.1 bar) overnight. The mixture was then filtered and the filtrate was flushed through a pad of silica gel, eluting with ethyl acetate, and then concentrated in vacuo. The crude solid was suspended in diethyl ether, sonicated, filtered and dried in vacuo to give 2.4 g (67%) of a faint green solid.

後処理

  1. filtrationThe mixture was then filtered
  2. customthe filtrate was flushed through a pad of silica gel
  3. washeluting with ethyl acetate
  4. concentrationconcentrated in vacuo
  5. customsonicated
  6. filtrationfiltered
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-49ab1e75f4764ea1903f26b672d22b5b
出典データセット
uspto-grants-2001_11
特許番号
US06313122B1

反応ノート

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