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Ethylamine → N-ethyl-4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyrimidin-2-amine

HRID 45883
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HRID 45883 반응식
[CH3:1][O:2][C:3]1[CH:33]=[CH:32][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([C:13]3[CH:18]=[CH:17][N:16]=[C:15](S(C)(=O)=O)[N:14]=3)[C:10]([C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([N+:29]([O-:31])=[O:30])[CH:24]=3)=[N:9]2)=[CH:5][CH:4]=1.[CH2:34]([NH2:36])[CH3:35]>O1CCOCC1.O>[CH2:34]([NH:36][C:15]1[N:14]=[C:13]([C:11]2[C:10]([C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([N+:29]([O-:31])=[O:30])[CH:24]=3)=[N:9][N:8]([CH2:7][C:6]3[CH:32]=[CH:33][C:3]([O:2][CH3:1])=[CH:4][CH:5]=3)[CH:12]=2)[CH:18]=[CH:17][N:16]=1)[CH3:35]
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참가 물질

5

반응물 2

HCID 6341EthylamineHCID 67184047HCID 67184047, 화합물

생성물 1

HCID 67184314N-ethyl-4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyrimidin-2-amine수율 94%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

450 mg (0.97 mmol) of 4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]-2-(methylsulfonyl)pyrimidine were dissolved in a mixture of 10 ml of dioxane and 5 ml of ethylamine 70% in water. The resulting solution was submitted to microwave irradiation in a sealed vial at 140° C. for 45 minutes. The solvent was then removed and the residue was partitioned between dichloromethane and aqueous sodium hydrogenocarbonate. The organic phase was then dried over sodium sulphate and evaporated to dryness. 391 mg (94%) of the title compound were obtained by trituration with diethylether.

후처리

  1. customirradiation in a sealed vial at 140° C. for 45 minutes
  2. customThe solvent was then removed
  3. customthe residue was partitioned between dichloromethane and aqueous sodium hydrogenocarbonate
  4. dry with materialThe organic phase was then dried over sodium sulphate
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-62ba743d0b6c4d45bf346836ac5f134c
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08541575B2

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