Methanol → Methyl 4,5-difluoro-2-nitrobenzoate

HRID 1172574ノート

反応式

HRID 1172574 の反応式
[F:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=1.OS(O)(=O)=O.[CH3:20]O>>[F:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([O:8][CH3:20])=[O:7])=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 42196304,5-Difluoro-2-nitrobenzoic acid

生成物 1

HCID 21928432Methyl 4,5-difluoro-2-nitrobenzoate

実験手順

To a solution of 4,5-difluoro-2-nitrobenzoic acid 1a (40.0 g, 196.947 mmol) in anhydrous MeOH (1.0 L), was added concentrated H2SO4 (60.0 mL) and the clear mixture was refluxed for 2 days. Then methanol was removed in vacuo and the residue was partitioned between EtOAc and water. The EtOAc extract was washed with brine, dried over with anhydrous. Na2SO4, and concentrated to yield the methyl 4,5-difluoro-2-nitrobenzoate 1b as a pale yellow solid, 39.71 g (93%).

後処理

  1. temperaturethe clear mixture was refluxed for 2 days
  2. customThen methanol was removed in vacuo
  3. customthe residue was partitioned between EtOAc and water
  4. extractionThe EtOAc extract
  5. washwas washed with brine
  6. customdried over with anhydrous
  7. concentrationNa2SO4, and concentrated

出典と根拠

ORDレコード
ord-296ed7a30b4b45768c7837a3414a43fc
出典データセット
uspto-grants-2010_11
特許番号
US07834023B2

反応ノート

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