2-Propenoic acid, 2-cyano-3-ethoxy-, ethyl ester → HCID 13654083, 화합물

HRID 280450노트

반응식

HRID 280450 반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:8]=[C:7]([Cl:9])[CH:6]=[CH:5][C:4]=1[NH:10][NH2:11].[CH2:14]([O:16][C:17](=[O:25])[C:18](=[CH:21]OCC)[C:19]#[N:20])[CH3:15]>C(O)(=O)C.O>[NH2:20][C:19]1[N:10]([C:4]2[CH:5]=[CH:6][C:7]([Cl:9])=[CH:8][C:3]=2[C:2]([F:1])([F:12])[F:13])[N:11]=[CH:21][C:18]=1[C:17]([O:16][CH2:14][CH3:15])=[O:25]

참가 물질

5

반응물 2

HCID 789432-Propenoic acid, 2-cyano-3-ethoxy-, ethyl esterHCID 2778240(4-Chloro-2-(trifluoromethyl)phenyl)hydrazine

생성물 1

HCID 13654083HCID 13654083, 화합물수율 85.9%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

A solution of 31.58 g of 2-(trifluoromethyl)-4-chlorophenylhydrazine and 27.92 g of ethyl(ethoxymethylene)cyanoacetate dissolved in 225 of acetic acid and 75 ml of water was heated on a steam bath for approximately 16 hours. The reaction mixture was cooled to room temperature and placed in the refrigerator. The precipitated solid was collected by filtration and combined with the solids isolated from the filtrate to provide 43 g of 5-amino-1-[2-(trifluoromethyl)-4-chlorophenyl]-1H-pyrazole-4-carboxylic acid, ethyl ester. MP=114°-116° C.

후처리

  1. temperaturewas heated on a steam bath for approximately 16 hours
  2. filtrationThe precipitated solid was collected by filtration
  3. customisolated from the filtrate

출처 및 근거

ORD 기록
ord-9726254e7b62442ab15a5e8aa42de1e7
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04589905

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