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

HRID 470360ノート

反応式

HRID 470360 の反応式
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

参加物

4

反応物 3

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

生成物 1

HCID 53419670Methyl 4-amino-2-fluoro-5-nitrobenzoate収率 69%

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4f3c42fec1894629a3d54dc0ae4bc438
出典データセット
uspto-grants-2014_01
特許番号
US08629147B2

反応ノート

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