Dimethylformamide → t-Butyl 4-(3-benzyl-4-chloro-3H-imidazo(4,5-c]pyridin-2-yl)piperazine-1-carboxylate

HRID 501444노트

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HRID 501444 반응식
[N:1]1([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.CN(C)C=O.[CH2:19]([N:26]1[C:30]2[C:31]([Cl:35])=[N:32][CH:33]=[CH:34][C:29]=2[NH:28][CH:27]1Cl)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C(OCC)(=O)C>[CH2:19]([N:26]1[C:30]2[C:31]([Cl:35])=[N:32][CH:33]=[CH:34][C:29]=2[N:28]=[C:27]1[N:4]1[CH2:5][CH2:6][N:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:2][CH2:3]1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 143452tert-Butyl piperazine-1-carboxylateHCID 574728443-Benzyl-2,4-dichloro-1,3-dihydroimidazo[4,5-c]pyridine

생성물 1

HCID 23070589t-Butyl 4-(3-benzyl-4-chloro-3H-imidazo(4,5-c]pyridin-2-yl)piperazine-1-carboxylate수율 14.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
150 °C

실험 절차

0.094 g of t-butyl piperazine-1-carboxylate was added to a 1 ml N,N-dimethylformamide solution of 0.127 g of 3-benzyl-2,4-dichloro-1,3-dihydroimidazo[4,5-c]pyridine, and the mixture was heated at 150° C. for two hours. 25 ml of ethyl acetate was added to the mixture, and the organic layer was washed three times with 10 ml of water and then with 10 ml of an aqueous solution saturated with sodium chloride. The organic liquid was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography. Thus, 0.029 g of the title compound was obtained from the fraction eluted with ethyl acetate-hexane (3:2).

후처리

  1. washthe organic layer was washed three times with 10 ml of water
  2. dry with materialThe organic liquid was dried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-18f80efefcc84a9fb204b98854d12c0f
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772226B2

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