Diethyl Ether → 1-(4-Pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxynaphthalene

HRID 1743034

반응식

HRID 1743034 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7]23O[CH:10]([C:11]4[C:16]2=[CH:15][C:14]([O:17][CH3:18])=[C:13]([O:19][CH3:20])[CH:12]=4)[C:9]([C:22]([O:24][CH3:25])=[O:23])=[C:8]3[C:26]([O:28][CH3:29])=[O:27])=[CH:3][CH:2]=1.FB(F)F.C(OCC)C>C(#N)C>[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:16]3[C:11](=[CH:12][C:13]([O:19][CH3:20])=[C:14]([O:17][CH3:18])[CH:15]=3)[CH:10]=[C:9]([C:22]([O:24][CH3:25])=[O:23])[C:8]=2[C:26]([O:28][CH3:29])=[O:27])=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 6356Boron trifluorideHCID 190062311-(4-Pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxy-1,4-epoxy-1,4-dihydronaphthalene

생성물 1

HCID 117286421-(4-Pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxynaphthalene수율 73%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1-(4-Pyridyl)- 2,3-bis(methoxycarbonyl)-6,7-dimethoxy-1,4-epoxy-1,4-dihydronaphthalene (3.0 g) and trifluoroborane.diethyl ether (1.95 g) are added to acetonitrile (100 ml), and the mixture is refluxed for 2 hours. The reaction solution is separated with a mixture of chloroform (300 ml) and aqueous sodium hydrogen carbonate solution (50 ml), and the organic layer is further washed with aqueous sodium hydrogen carbonate solution, dried, and concentrated. The resulting residue is washed with a small amount of diethyl ether to give 1-(4-pyridyl)-2,3-bis(methoxy-carbonyl)-6,7-dimethoxynaphthalene (2.1 g) as crystal.

후처리

  1. temperaturethe mixture is refluxed for 2 hours
  2. customThe reaction solution is separated with a mixture of chloroform (300 ml) and aqueous sodium hydrogen carbonate solution (50 ml)
  3. washthe organic layer is further washed with aqueous sodium hydrogen carbonate solution
  4. customdried
  5. concentrationconcentrated
  6. washThe resulting residue is washed with a small amount of diethyl ether

출처 및 근거

ORD 기록
ord-1ac07c276e6c413681a20eb07e24fb5f
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05342941

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