Methanol → HCID 57749798、化合物

HRID 553780ノート

反応式

HRID 553780 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 solution was washed with brine, dried over NaSO4, 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 solution was washed with brine
  5. dry with materialdried over NaSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2d17a5eac188416fb8a9d27cfd3c4d9e
出典データセット
uspto-grants-2011_11
特許番号
US08048905B2

反応ノート

読み込み中…