2-Chloro-4-fluoro-5-nitrobenzoic Acid → 5-Amino-2-chloro-4-fluorobenzoic acid

HRID 22635노트

반응식

HRID 22635 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([N+:12]([O-])=O)=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]>C(O)(=O)C.O.C(OCC)(=O)C.[Fe]>[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([NH2:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

6

반응물 1

HCID 72108282-Chloro-4-fluoro-5-nitrobenzoic Acid

생성물 1

HCID 120567845-Amino-2-chloro-4-fluorobenzoic acid

시약·촉매·용매 4

HCID 23925Iron촉매HCID 176Acetic Acid용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 2-chloro-4-fluoro-5-nitrobenzoic acid (18.0 g, 0.0824 mol) in 75 ml of acetic acid was heated at reflux temperature. Iron powder (18.4 g, 0.328 mol) was added in several portions and the resulting suspension was cooled to room temperature and diluted with water and ethyl acetate. The mixture was filtered and the filtrate was saved. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to afford the title compound as a tan solid. Yield: 9.00 g (58.1%); mp.: 153-155° C.; identified by NMR and mass spectral analysis.

후처리

  1. temperatureat reflux temperature
  2. filtrationThe mixture was filtered
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1151058879a045ecbe8c8101f445d1c7
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849618B2

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