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Water → 2-bromo-4-(6,7-dimethoxy-2-methoxycarbonylmethylphthalazin-1(2H)-on-4-yl)pyridine

HRID 1739427
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HRID 1739427 반응식
[Br:1][C:2]1[CH:7]=[C:6]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:20][CH3:21])=[C:15]([O:18][CH3:19])[CH:16]=3)[C:11](=[O:22])[NH:10][N:9]=2)[CH:5]=[CH:4][N:3]=1.[H-].[Na+].Br[CH2:26][C:27]([O:29][CH3:30])=[O:28].O>CN(C)C=O>[Br:1][C:2]1[CH:7]=[C:6]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:20][CH3:21])=[C:15]([O:18][CH3:19])[CH:16]=3)[C:11](=[O:22])[N:10]([CH2:26][C:27]([O:29][CH3:30])=[O:28])[N:9]=2)[CH:5]=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 60984Methyl bromoacetateHCID 218408052-bromo-4-(6,7-dimethoxyphthalazin-1(2H)-on-4-yl)pyridine

생성물 1

HCID 218408072-bromo-4-(6,7-dimethoxy-2-methoxycarbonylmethylphthalazin-1(2H)-on-4-yl)pyridine

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

To a solution of 2-bromo-4-(6,7-dimethoxyphthalazin-1(2H)-on-4-yl)pyridine (362 mg) in dimethylformamide (2 ml) is added sodium hydride (48 mg, 62.4% in oil,) with ice-cooling under nitrogen atmosphere, and the mixture is stirred at room temperature for 30 minutes. To the mixture is methyl bromoacetate (0.11 ml) under ice-cooling, and the mixture is stirred for 15 minutes. To the mixture is added water, and the mixture is extracted with ethyl acetate. The extract is washed, dried, and concentrated to give 2-bromo-4-(6,7-dimethoxy-2-methoxycarbonylmethylphthalazin-1(2H)-on-4-yl)pyridine (390 mg).

후처리

  1. temperaturecooling under nitrogen atmosphere
  2. temperaturecooling
  3. stirringthe mixture is stirred for 15 minutes
  4. extractionthe mixture is extracted with ethyl acetate
  5. washThe extract is washed
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2e4e22712c304cbb871830e38f156e51
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05965730

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