Methanol → Methyl 4-amino-2-fluoro-5-nitrobenzoate

HRID 470360노트

반응식

HRID 470360 반응식
S(=O)(=O)(O)O.[NH2:6][C:7]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[C:9]([F:19])[CH:8]=1.[CH3:20]O>>[NH2:6][C:7]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][C:10]([C:11]([O:13][CH3:20])=[O:12])=[C:9]([F:19])[CH:8]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 597853374-Amino-2-fluoro-5-nitrobenzoic acid

생성물 1

HCID 53419670Methyl 4-amino-2-fluoro-5-nitrobenzoate수율 69%

실험 절차

Sulfuric acid (10 mL) was added to a solution of 4-amino-2-fluoro-5-nitrobenzoic acid ammoniate (10 g, 46 mmol) in methanol (100 mL) and refluxed for 30 h. The solution was cooled to ambient temperature and the solid thus obtained was collected by filtration, washed with hexanes, and dried in vacuo at 40° C. for 14 h to afford the desired methyl 4-amino-2-fluoro-5-nitrobenzoate as a yellow solid (6.84 g, 31.9 mmol, 69%). 1H NMR (MeOD) δ 8.62-8.58 (m, 1H), 6.63-6.59 (m, 1H).

후처리

  1. temperaturerefluxed for 30 h
  2. customthe solid thus obtained
  3. filtrationwas collected by filtration
  4. washwashed with hexanes
  5. customdried in vacuo at 40° C. for 14 h

출처 및 근거

ORD 기록
ord-4f3c42fec1894629a3d54dc0ae4bc438
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629147B2

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