Sodium Hydroxide → 4-(1-methyl-1H-pyrazol-4-yl)benzoic acid

HRID 2307349노트

반응식

HRID 2307349 반응식
[CH3:1][N:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=2)[CH:4]=[N:3]1.[Mn]([O-])(=O)(=O)=[O:15].[K+].[OH-:20].[Na+]>>[CH3:1][N:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([C:13]([OH:15])=[O:20])=[CH:9][CH:8]=2)[CH:4]=[N:3]1

참가 물질

4

반응물 3

HCID 14798Sodium HydroxideHCID 516875Potassium PermanganateHCID 43190701-Methyl-4-(4-methylphenyl)-1H-pyrazole

생성물 1

HCID 226054524-(1-methyl-1H-pyrazol-4-yl)benzoic acid

실험 절차

A mixture of 1-methyl-4-(4-methylphenyl)-1H-pyrazole (1.70 g), potassium permanganate (9.70 g), and 1 N sodium hydroxide (100 ml) was refluxed for 18 hours. The suspension was filtered through diatomaceous earth and cooled. The aqueous solution was extracted with dichloromethane which was discarded. The aqueous solution was acidified to pH 5.5. The resultant precipitate was difficult to filter and was thus extracted with dichloromethane. After evaporation of the solvent, the resulting solid was recrystallized from acetone to yield the title compound (0.60 g), m.p. 274-275° C.; MS m/z: 202 (M)+.

후처리

  1. temperaturewas refluxed for 18 hours
  2. filtrationThe suspension was filtered through diatomaceous earth
  3. temperaturecooled
  4. extractionThe aqueous solution was extracted with dichloromethane which
  5. filtrationto filter
  6. extractionwas thus extracted with dichloromethane
  7. customAfter evaporation of the solvent
  8. customthe resulting solid was recrystallized from acetone

출처 및 근거

ORD 기록
ord-ff149dcc71294afc9e7b5e6aeafef8ad
출처 데이터셋
uspto-grants-2004_12
특허 번호
US06831079B1

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