Sodium Hydroxide → 2-Methoxy-3-nitrobenzoic acid

HRID 351343ノート

反応式

HRID 351343 の反応式
[OH-].[Na+].[CH3:3][O:4][C:5]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=[CH:11][C:6]=1[C:7]([O:9]C)=[O:8]>CO>[CH3:3][O:4][C:5]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=[CH:11][C:6]=1[C:7]([OH:9])=[O:8]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 590805Methyl 2-methoxy-3-nitrobenzoate

生成物 1

HCID 120151952-Methoxy-3-nitrobenzoic acid収率 94.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

1N Sodium hydroxide was added to a solution (50 ml) of methyl 2-methoxy-3-nitrobenzoate (4.96 g, 23.5 mmol) in methanol and the mixture was stirred at 50° C. for 2 hrs. Methanol was evaporated under reduced pressure and water was added. The aqueous layer was acidified with 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The obtained residue was recrystallized from hexane-ethyl acetate to give the title compound (4.37 g) as pale-yellow crystals. melting point: 224–226° C.

後処理

  1. customMethanol was evaporated under reduced pressure and water
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe obtained residue was recrystallized from hexane-ethyl acetate

出典と根拠

ORDレコード
ord-32a364d3ba2d434ca707fb8ad0c8b738
出典データセット
uspto-grants-2007_02
特許番号
US07183415B2

反応ノート

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