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

HRID 1731260ノート

反応式

HRID 1731260 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-92765eba177d4875b6ce732748c3c743
出典データセット
uspto-grants-1986_11
特許番号
US04620865

反応ノート

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