Potassium Carbonate → 4-methyl-3-(4-penten-1-yl)-5-phenyl-4H-1,2,4-triazole

HRID 550530노트

반응식

HRID 550530 반응식
Cl.[CH3:2][NH:3][C:4](=NC)[CH2:5][CH2:6][CH2:7][CH:8]=[CH2:9].C([O-])([O-])=O.[K+].[K+].[C:18]([NH:26][NH2:27])(=O)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>CO>[CH3:2][N:3]1[C:18]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:26][N:27]=[C:4]1[CH2:5][CH2:6][CH2:7][CH:8]=[CH2:9]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 11955BenzoylhydrazineHCID 86630240N,N'-dimethyl-5-hexenimidamide hydrochloride

생성물 1

HCID 576918864-methyl-3-(4-penten-1-yl)-5-phenyl-4H-1,2,4-triazole수율 0%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of N,N′-dimethyl-5-hexenimidamide hydrochloride (3.1Mmol) in MeOH (20 ml) were added K2CO3 (3.1Mmol) and benzhydrazide (3.1Mmol). The solution was heated to reflux for 24 h. Volatiles were evaporated in vacuo, the crude dissolved in DCM, washed with water and dried over Na2SO4. After filtration and concentration to dryness in vacuo, the crude was purified by column chromatography (DCM:MeOH=98 to 2) to give 196 mg of the title compound.

후처리

  1. temperatureThe solution was heated
  2. temperatureto reflux for 24 h
  3. customVolatiles were evaporated in vacuo
  4. dissolutionthe crude dissolved in DCM
  5. washwashed with water
  6. dry with materialdried over Na2SO4
  7. filtrationAfter filtration and concentration to dryness in vacuo
  8. customthe crude was purified by column chromatography (DCM:MeOH=98 to 2)

출처 및 근거

ORD 기록
ord-872fc588945d4b25b5d6cca8b78bfcdb
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947683B2

반응 노트

불러오는 중…