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Dimethylformamide → HCID 19603281, 화합물

HRID 1604599
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HRID 1604599 반응식
[Cl:1][C:2]1[C:20]([NH:21][C:22](=[O:29])[CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26])=[CH:19][CH:18]=[C:17]([Cl:30])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:15]=1[N:14]=[C:13]([CH3:16])[CH:12]=[CH:11]2.IC.[CH3:33]N(C)C=O.[H-].[Na+]>C(OCC)(=O)C>[Cl:1][C:2]1[C:20]([N:21]([C:22](=[O:29])[CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26])[CH3:33])=[CH:19][CH:18]=[C:17]([Cl:30])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:15]=1[N:14]=[C:13]([CH3:16])[CH:12]=[CH:11]2
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참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 196032998-[2,6-Dichloro-3-(3-methoxycarbonylpropionylamino)benzyloxy]-2-methylquinoline

생성물 1

HCID 19603281HCID 19603281, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 8-[2,6-dichloro-3-(3-methoxycarbonylpropionylamino)benzyloxy]-2-methylquinoline (447 mg), iodomethane (0.1 ml) and dimethylformamide (5.0 ml) was added sodium hydride (60% in oil, 44 mg) under ice-water cooling. After stirring for 2 hours at the same temperature, the reaction mixture was diluted with ethyl acetate and washed with water twice. The organic layer was dried over magnesium sulfate and evaporated in vacuo. The residue was purified by a column chromatography eluted with chloroform to give 8-[2,6-dichloro-3-[N-(3-methyoxycarbonylpropionyl)-N-methylamino]benzyloxy]-2-methylquinoline (310 mg) as a pale yellow oil.

후처리

  1. washwashed with water twice
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. customevaporated in vacuo
  4. customThe residue was purified by a column chromatography
  5. washeluted with chloroform

출처 및 근거

ORD 기록
ord-f94b1f8183874f9ea01692849d8eeb55
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05994368

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