Water → 5-Amino-3-(methylthio)-1-(2,4,6-trichlorophenyl)pyrazole-4-carboxamide

HRID 324375

반응식

HRID 324375 반응식
[CH3:1][S:2][C:3](=[C:6]([C:10]#[N:11])[C:7]([NH2:9])=[O:8])SC.[Cl:12][C:13]1[CH:18]=[C:17]([Cl:19])[CH:16]=[C:15]([Cl:20])[C:14]=1[NH:21][NH2:22].O>CO>[NH2:11][C:10]1[N:21]([C:14]2[C:13]([Cl:12])=[CH:18][C:17]([Cl:19])=[CH:16][C:15]=2[Cl:20])[N:22]=[C:3]([S:2][CH3:1])[C:6]=1[C:7]([NH2:9])=[O:8]

참가 물질

5

반응물 3

HCID 962WaterHCID 79234(2,4,6-Trichlorophenyl)hydrazineHCID 27477462-Cyano-3,3-bis(methylthio)acrylamide

생성물 1

HCID 113025915-Amino-3-(methylthio)-1-(2,4,6-trichlorophenyl)pyrazole-4-carboxamide수율 81.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of bis(methythio)methylenecyanoacetamide (7.800 g, 50 mmol) and 2,4,6-trichlorophenylhydrazine (10.575 g, 50 mmol) in 250 ml of methanol was heated at reflux for 2.5 hours. The mixture was cooled and water was added. Precipitate formed and filtered to give 14.323 g (81.5% yield) of the title compound as a white solid. 1H NMR(CDCl3): 2.6 (s,3H), 5.5(brs, 2H), 7.5(s,2H) ppm. Recrystallization of a small portion of the solid from chloroform gave white crystals; m. p. 198-199° C. Anal. Calc. for C11H9Cl3N4OS: C, 37.57; H, 2.58; N, 15.93; Found: C, 37.54; H, 2.51; N, 15.73.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2.5 hours
  3. temperatureThe mixture was cooled
  4. customPrecipitate formed
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-c13c5fd8e8314a288ea8f87bcf3cb292
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218397B1

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