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

HRID 427712노트

반응식

HRID 427712 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-49ab1e75f4764ea1903f26b672d22b5b
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313122B1

반응 노트

불러오는 중…