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

HRID 550546노트

반응식

HRID 550546 반응식
[CH3:1][C:2]([CH3:10])([CH2:7][CH:8]=[CH2:9])[C:3]([NH:5][NH2:6])=O.C([O-])([O-])=O.[K+].[K+].Cl.[CH3:18][NH:19][C:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=NC>CN1C(=O)CCC1>[CH3:1][C:2]([C:3]1[N:19]([CH3:18])[C:20]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:6][N:5]=1)([CH3:10])[CH2:7][CH:8]=[CH2:9]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 12382386N,N'-dimethylbenzenecarboximidamide hydrochlorideHCID 576918522,2-Dimethyl-4-pentenohydrazide

생성물 1

HCID 576918753-(1,1-dimethyl-3-buten-1-yl)-4-methyl-5-phenyl-4H-1,2,4-triazole수율 32.1%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
240 °C

실험 절차

To a solution of 2,2-dimethyl-4-pentenohydrazide (360 mg) in NMP(2.5 ml) were added K2CO3 (348 mg) and N,N′-dimethylbenzenecarboximidamide hydrochloride (463 mmol). The solution was heated to the microwave at 240° C. for 30 minutes. 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. MS (m/z): 242[MH]+.

후처리

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

출처 및 근거

ORD 기록
ord-b5aa1ae7db544f1593f7c7c18c27cefc
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947683B2

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