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

HRID 1799021ノート

反応式

HRID 1799021 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 20v/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 20v/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-580bfe9b8add468298624df49db273e5
出典データセット
uspto-grants-2013_01
特許番号
US08343994B2

反応ノート

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