3-(Oxiran-2-yl)pyridine → HCID 18007277, 화합물

HRID 1351909노트

반응식

HRID 1351909 반응식
[O:1]1[CH2:3][CH:2]1[C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1.[CH2:10]([NH:17][CH:18]1[CH2:24][CH2:23][CH2:22][C:21]2[CH:25]=[CH:26][C:27]([O:29][CH3:30])=[CH:28][C:20]=2[CH2:19]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C(O)C>[CH2:10]([N:17]([CH2:3][CH:2]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)[OH:1])[CH:18]1[CH2:24][CH2:23][CH2:22][C:21]2[CH:25]=[CH:26][C:27]([O:29][CH3:30])=[CH:28][C:20]=2[CH2:19]1)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

4

반응물 2

HCID 133195613-(Oxiran-2-yl)pyridineHCID 18007303HCID 18007303, 화합물

생성물 1

HCID 18007277HCID 18007277, 화합물수율 11%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Under nitrogen, a solution of 3-oxiranylpyridine (1.9 g) and N-benzyl-(3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)amine (3.3 g) in ethanol (15 ml) was refluxed for 5 hours. After removal of ethanol in vacuo, the residue was dissolved into a mixture of aqueous sodium hydrogencarbonate and ethyl acetate. After separation, the organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel (chloroform:methanol=20:1) to give 2-[N-benzyl-N-(3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)amino]-1-(pyridin-3-yl)ethanol (520 mg).

후처리

  1. customAfter removal of ethanol in vacuo
  2. dissolutionthe residue was dissolved into a mixture of aqueous sodium hydrogencarbonate and ethyl acetate
  3. customAfter separation
  4. washthe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel (chloroform:methanol=20:1)

출처 및 근거

ORD 기록
ord-14a3cf1a75444593bdbd099c522bf0cd
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217706B2

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