Sodium Hydroxide → 2'-Methyl-biphenyl-2,4'-dicarboxylic acid

HRID 541140ノート

反応式

HRID 541140 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([O:10]C)=[O:9])[CH:5]=[CH:4][C:3]=1[C:12]1[C:13]([C:18]([O:20]CC)=[O:19])=[CH:14][CH:15]=[CH:16][CH:17]=1.[OH-].[Na+]>C(O)C>[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][C:3]=1[C:12]1[C:13]([C:18]([OH:20])=[O:19])=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 594926732-Ethyl 4'-methyl 2'-methyl-biphenyl-2,4'-dicarboxylate

生成物 1

HCID 594924972'-Methyl-biphenyl-2,4'-dicarboxylic acid収率 95%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2-ethyl 4′-methyl 2′-methyl-biphenyl-2,4′-dicarboxylate (2.404 g), ethanol (12 ml) and 4N aqueous sodium hydroxide solution (6 ml) was stirred at 100° C. overnight. After completion of the reaction, the reaction mixture was concentrated under reduced pressure, and water (50 ml) was added to the obtained residue. This mixture was adjusted to pH 1 with 6N hydrochloric acid (5 ml), ethanol (10 ml) was added, and the mixture was stirred at room temperature for 10 min. This suspension was filtered, the obtained solid was washed with 20 v/v % ethanol-water (10 ml), air-dried, and dried under reduced pressure at 80° C. to give the title compound (1.957 g, 95%).

後処理

  1. customAfter completion of the reaction
  2. concentrationthe reaction mixture was concentrated under reduced pressure, and water (50 ml)
  3. additionwas added to the obtained residue
  4. additionwas added
  5. stirringthe mixture was stirred at room temperature for 10 min
  6. filtrationThis suspension was filtered
  7. washthe obtained solid was washed with 20 v/v % ethanol-water (10 ml)
  8. customair-dried
  9. customdried under reduced pressure at 80° C.

出典と根拠

ORDレコード
ord-8a453cca6f3343f991c55d8ca946965a
出典データセット
uspto-grants-2014_10
特許番号
US08871934B2

反応ノート

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