Potassium Hydroxide → 1H-Pyrazole-4-carboxylic acid, 5-(aminocarbonyl)-1-(4-methylphenyl)-

HRID 867381노트

반응식

HRID 867381 반응식
[C:1]([C:3]1[N:7]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)[N:6]=[CH:5][C:4]=1[C:15]([O:17]CC)=[O:16])#[N:2].[OH-:20].[K+]>O>[C:15]([C:4]1[CH:5]=[N:6][N:7]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)[C:3]=1[C:1]([NH2:2])=[O:20])([OH:17])=[O:16]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 13772970Ethyl 5-cyano-1-(4-methylphenyl)-1H-pyrazole-4-carboxylate

생성물 1

HCID 1637161H-Pyrazole-4-carboxylic acid, 5-(aminocarbonyl)-1-(4-methylphenyl)-

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To 10 g. of ethyl 5-cyano-1-(4-methylphenyl)-4-pyrazolecarboxylate was added 5.6 g. of potassium hydroxide and 200 ml. of water followed by enough water to cause solution. The mixture was stirred under reflux for 8hours and allowed to stand for 3 days. It was then poured over ice, made acid and filtered. The solids from the filtration were heated in 100 ml. of ethyl acetate, and the undissolved solid was separated, dried and identified as 4.25 g. of the desired product, m.p. 260° dec. The product was identified by nuclear magnetic resonance analysis in DMSOd6. δ2.36 (s, 3), methyl; 7.32 (d, 2), aromatic; 7.45 (d, 2), aromatic; 8.01 (s, 1), pyrazole; 7.91 (s, 1), carboxamide; 8.33 (s, 1), carboxamide.

후처리

  1. temperatureunder reflux for 8hours
  2. additionIt was then poured over ice
  3. filtrationfiltered
  4. filtrationThe solids from the filtration
  5. temperaturewere heated in 100 ml
  6. customof ethyl acetate, and the undissolved solid was separated
  7. customdried

출처 및 근거

ORD 기록
ord-5868a1ee510c42739b17dc774485354b
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04775409

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