Dimethylformamide → 2-[(4-Methoxyphenyl)amino]benzoic acid

HRID 464786

反応式

HRID 464786 の反応式
Cl[C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH3:11][O:12][C:13]1[CH:19]=[CH:18][C:16]([NH2:17])=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[CH3:11][O:12][C:13]1[CH:19]=[CH:18][C:16]([NH:17][C:2]2[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=2[C:4]([OH:6])=[O:5])=[CH:15][CH:14]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7732P-AnisidineHCID 83742-Chlorobenzoic AcidHCID 11430Potassium Carbonate

生成物 1

HCID 2029182-[(4-Methoxyphenyl)amino]benzoic acid収率 76%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 52 g (0.33 mole) of 2-chlorobenzoic acid, 82 g (0.66 mole) of 4-methoxyaniline, 46 g (0.33 mole) of potassium carbonate, 5 g (0.025 mole) of cupric acetate and 150 ml of dimethylformamide was heated at reflux for two hours. The reaction mixture was cooled, 300 ml of water added and the mixture filtered. The filtrate was acidified with 50 ml of 6N hydrochloric acid, and the resulting solid was collected by filtration and recrystallized from acetonitrile to give 61 g of 2-(4-methoxyphenylamino)benzoic acid.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for two hours
  3. temperatureThe reaction mixture was cooled
  4. filtrationthe mixture filtered
  5. filtrationthe resulting solid was collected by filtration
  6. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-e6d807f084a54bd7b8b146c779fc9dae
出典データセット
uspto-grants-1985_10
特許番号
US04549016

関連ノート

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