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

HRID 1799021노트

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HRID 1799021 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
100 °C

실험 절차

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%).

후처리

  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.

출처 및 근거

ORD 기록
ord-580bfe9b8add468298624df49db273e5
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08343994B2

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