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(2E)-2-[(3-bromo-4-pyridyl)-methylene]-6-methoxy-tetralin-1-one → 2-[(3-Bromo-4-pyridyl)methyl]-6-methoxy-tetralin-1-one

HRID 2207194
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인쇄 미리보기

반응식

HRID 2207194 반응식
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1/[CH:8]=[C:9]1/[C:10](=[O:21])[C:11]2[C:16]([CH2:17][CH2:18]/1)=[CH:15][C:14]([O:19][CH3:20])=[CH:13][CH:12]=2>CCO.[Pt]>[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH2:8][CH:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([O:19][CH3:20])[CH:15]=2)[C:10]1=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 118557971(2E)-2-[(3-bromo-4-pyridyl)-methylene]-6-methoxy-tetralin-1-one

생성물 1

HCID 1185580372-[(3-Bromo-4-pyridyl)methyl]-6-methoxy-tetralin-1-one수율 99.4%

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 702Ethanol용매

실험 절차

Pt/C (5 wt % loading, 200 mg) was added to a stirred solution of the compound 87 (2.0 g, 5.81 mmol) in EtOH (58 mL) at room temperature. The resulting suspension was stirred for 4 hours under H2 atmosphere (1 atm) then filtered over Celite, rinsed with dichloromethane and concentrated to dryness. The crude residue was purified by column chromatography on SiO2 (gradient of EtOAc in petroleum ether) to afford the title compound 99 (Yield 2.0 g, 99%).

후처리

  1. filtrationthen filtered over Celite
  2. washrinsed with dichloromethane
  3. concentrationconcentrated to dryness
  4. customThe crude residue was purified by column chromatography on SiO2 (gradient of EtOAc in petroleum ether)

출처 및 근거

ORD 기록
ord-f281a1d249bd470aaa551745148ce49c
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376387B2

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