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

HRID 395862노트

반응식

HRID 395862 반응식
[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]

참가 물질

5

반응물 1

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

생성물 1

HCID 121506942-Amino-5-chloro-N-2-pyridinylbenzamide수율 67.3%

시약·촉매·용매 3

HCID 935Nickel촉매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-25c8482337784a1281f368af2c822003
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06605626B2

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