Potassium Carbonate → Ethyl 5-amino-1-(3-chlorophenyl)-1H-pyrazole-4-carboxylate

HRID 1731260노트

반응식

HRID 1731260 반응식
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([NH:9][NH2:10])[CH:6]=[CH:7][CH:8]=1.[CH2:11]([O:13][C:14](=[O:22])[C:15](=[CH:18]OCC)[C:16]#[N:17])[CH3:12].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:17][C:16]1[N:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([Cl:2])[CH:4]=2)[N:10]=[CH:18][C:15]=1[C:14]([O:13][CH2:11][CH3:12])=[O:22]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 75331m-Chlorophenylhydrazine hydrochlorideHCID 789432-Propenoic acid, 2-cyano-3-ethoxy-, ethyl ester

생성물 1

HCID 757292Ethyl 5-amino-1-(3-chlorophenyl)-1H-pyrazole-4-carboxylate수율 67%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 53.7 g of (3-chlorophenyl)hydrazine hydrochloride, 50.8 g of ethyl(ethoxymethylene)cyanoacetate and 41.4 g of potassium carbonate in 500 ml of ethanol was refluxed for 20 hours. The solution was poured into ice water. The precipitated solid was collected by filtration, dried and recrystallized from ethanol/water to provide 53.0 g of 5-amino-1-(3-chlorophenyl)-1H-pyrazole-4-carboxylic acid, ethyl ester. Yield 67%. mp=115°-117° C.

후처리

  1. filtrationThe precipitated solid was collected by filtration
  2. customdried
  3. customrecrystallized from ethanol/water

출처 및 근거

ORD 기록
ord-92765eba177d4875b6ce732748c3c743
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04620865

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