Methanol → HCID 57749798、化合物

HRID 77763ノート

反応式

HRID 77763 の反応式
[F:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([I:14])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].O=S(Cl)Cl.[CH3:19]O>>[CH3:19][O:5][C:4](=[O:6])[C:3]1[CH:7]=[C:8]([I:14])[CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:2]=1[F:1]

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 57749803HCID 57749803、化合物

生成物 1

HCID 57749798HCID 57749798、化合物収率 96%

実験手順

2-Fluoro-5-iodo-3-nitro-benzoic acid (2.0 g, 6.43 mmol) and SOCl2 (918 mg, 7.72 mmol) were added to 20 mL MeOH, and the mixture was refluxed for two hours and then cooled to room temperature. Solvent was evaporated under reduced pressure and the residue was dissolved in EtOAa. The EtOAc slolution was washed with brine, dried over NasSO4, filtered and concentrated under reduced pressure to give 2.0 g (96%) of 2-fluoro-5-iodo-3-nitro-benzoic acid methyl ester.

後処理

  1. temperaturethe mixture was refluxed for two hours
  2. customSolvent was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in EtOAa
  4. washThe EtOAc slolution was washed with brine
  5. customdried over NasSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a00ea54da970414c8701fa302f601d74
出典データセット
uspto-grants-2014_09
特許番号
US08841336B2

反応ノート

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