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Sodium Hydroxide → 5-Methylbiphenyl-2-carboxylic acid

HRID 2121201
ノート
印刷プレビュー

反応式

HRID 2121201 の反応式
C[O:2][C:3](=[O:17])[C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[CH:6][C:5]=1[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[OH-].[Na+]>CO>[CH3:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([OH:17])=[O:2])=[C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 18474515HCID 18474515、化合物

生成物 1

HCID 154962685-Methylbiphenyl-2-carboxylic acid収率 97.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 4-methyl-2-phenylbenzoic acid methyl ester (1.83 g, 8.09 mmol), prepared as in Example 227A, in methanol (16 mL) was added aqueous 4N sodium hydroxide (5 mL) and the reaction mixture was stirred for 60 hours, after which additional aqueous 4N sodium hydroxide (5 mL) was added and the mixture was heated at reflux for 5 hours. The reaction mixture was cooled to ambient temperature and the methanol was evaporated in vacuo. The aqueous residue was acidified with 4N sulfuric acid and extracted with ethyl acetate (3×). The combined organic extracts were dried, filtered, and concentrated in vacuo to give 4-methyl-2-phenylbenzoic acid (1.67 g) as a white solid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 5 hours
  3. customthe methanol was evaporated in vacuo
  4. extractionextracted with ethyl acetate (3×)
  5. customThe combined organic extracts were dried
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-09d8500c06cd409896b6f4fcfa991776
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06693123B2

反応ノート

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