2-Propenoic acid, 2-cyano-3-ethoxy-, ethyl ester → 5-Amino-4-ethoxycarbonyl-1-(2,3,5,6-tetrafluoro-4-trifluoromethyl-phenyl)-pyrazole

HRID 2232175노트

반응식

HRID 2232175 반응식
[F:1][C:2]1[C:7]([F:8])=[C:6]([C:9]([F:12])([F:11])[F:10])[C:5]([F:13])=[C:4]([F:14])[C:3]=1[NH:15][NH2:16].C(O[CH:20]=[C:21]([C:27]#[N:28])[C:22]([O:24][CH2:25][CH3:26])=[O:23])C>C(O)C>[NH2:28][C:27]1[N:15]([C:3]2[C:2]([F:1])=[C:7]([F:8])[C:6]([C:9]([F:12])([F:11])[F:10])=[C:5]([F:13])[C:4]=2[F:14])[N:16]=[CH:20][C:21]=1[C:22]([O:24][CH2:25][CH3:26])=[O:23]

참가 물질

4

반응물 2

HCID 789432-Propenoic acid, 2-cyano-3-ethoxy-, ethyl esterHCID 298179(alpha,alpha,alpha,2,3,5,6-Heptafluoro-p-tolyl)hydrazine

생성물 1

HCID 139337085-Amino-4-ethoxycarbonyl-1-(2,3,5,6-tetrafluoro-4-trifluoromethyl-phenyl)-pyrazole수율 87.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

40 g (0.161 mol) of 2,3,5,6-tetrafluoro-4-trifluoromethylphenylhydrazine and 27.8 g (0.161 mol) of ethyl ethoxymethylenecyanoacetate are dissolved in 70 ml of ethanol and the solution is warmed under reflux for 10 hours. The solvent is distilled off in vacuo, the residue is suspended in 100 ml of diethyl ether, the suspension is filtered and the solid is dried. 52.2 g (87.4% of theory) of 5-amino-4-ethoxycarbonyl-1-(2,3,5,6-tetrafluoro-4-trifluoromethyl-phenyl)-pyrazole of melting point 175° C.-176° C. are obtained.

후처리

  1. temperaturethe solution is warmed
  2. temperatureunder reflux for 10 hours
  3. distillationThe solvent is distilled off in vacuo
  4. filtrationthe suspension is filtered
  5. customthe solid is dried

출처 및 근거

ORD 기록
ord-6a2863a51dcf42b8814ae7265b38d15a
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04787930

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