Ethanol → 3-(2,6-Difluorophenyl)-6-methyl-[1,2,4]triazine

HRID 2085925노트

반응식

HRID 2085925 반응식
[CH3:1]C(C=O)=O.C(OC([NH:13][NH:14][C:15]([C:17]1[C:22]([F:23])=[CH:21][CH:20]=[CH:19][C:18]=1[F:24])=[NH:16])=O)(C)(C)C.[CH2:25](O)[CH3:26]>>[F:24][C:18]1[CH:19]=[CH:20][CH:21]=[C:22]([F:23])[C:17]=1[C:15]1[N:14]=[N:13][C:25]([CH3:26])=[CH:1][N:16]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 880MethylglyoxalHCID 178454364HCID 178454364, 화합물

생성물 1

HCID 227270203-(2,6-Difluorophenyl)-6-methyl-[1,2,4]triazine

실험 절차

1.89 g of methylglyoxal (40% in water) are added to 2.71 g of N′-[(2,6-difluorophenyl)-iminomethyl]-hydrazinecarboxylic acid tert-butyl ester in 30 ml of ethanol and stirring is carried out at room temperature for 16 h. The reaction mixture is then concentrated, and the residue is taken up in 20 ml of formic acid and stirring is continued at room temperature for 5 h. The reaction mixture is concentrated by evaporation; the residue is again dissolved in 20 ml of ethanol, boiled under reflux for 2 h, then concentrated and purified by means of column chromatography. In this way 3-(2,6-difluorophenyl)-6-methyl-[1,2,4]triazine having a melting point of 90-93° C. is obtained.

후처리

  1. concentrationThe reaction mixture is then concentrated
  2. stirringstirring
  3. waitis continued at room temperature for 5 h
  4. concentrationThe reaction mixture is concentrated by evaporation
  5. dissolutionthe residue is again dissolved in 20 ml of ethanol
  6. temperatureunder reflux for 2 h
  7. concentrationconcentrated
  8. custompurified by means of column chromatography

출처 및 근거

ORD 기록
ord-3da89dad3b164d138b7a492d14a6e5f3
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06723720B2

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