N,N-二甲基甲酰胺 → 5-Bromo-2-(2,2-diethoxyethoxy)pyrimidine

HRID 15063

反应方程式

HRID 15063 反应方程式
[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5][OH:6])[CH3:2].C(=O)([O-])[O-].[Cs+].[Cs+].CN(C=O)C.[Br:21][C:22]1[CH:23]=[N:24][C:25](Cl)=[N:26][CH:27]=1>O>[Br:21][C:22]1[CH:23]=[N:24][C:25]([O:6][CH2:5][CH:4]([O:7][CH2:8][CH3:9])[O:3][CH2:1][CH3:2])=[N:26][CH:27]=1

参与物

6

反应物 4

HCID 6228N,N-二甲基甲酰胺HCID 10796碳酸氢铯HCID 121292,2-二乙氧基乙醇HCID 6066655-溴-2-氯嘧啶

产物 1

HCID 684312375-Bromo-2-(2,2-diethoxyethoxy)pyrimidine收率 94.2%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

2,2-Diethoxyethanol (1.6 g) and cesium carbonate (5.8 g) were added to DMF solution (10 mL) of 5-bromo-2-chloropyrimidine (1.15 g), and stirred at room temperature for 12 hours. After addition of water, the reaction liquid was extracted with ethyl acetate and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the residue was purified on silica gel column chromatography (C-200; ethyl acetate:hexane=1:9-1:4) to provide the title compound (1.63 g, 94%).

后处理

  1. customthe reaction liquid
  2. extractionwas extracted with ethyl acetate
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationConcentrating the solvent under reduced pressure
  5. customthe residue was purified on silica gel column chromatography (C-200; ethyl acetate:hexane=1:9-1:4)

来源与证据

ORD记录
ord-1ba2013ec1264fe3af9606dd2c8fb343
来源数据集
uspto-grants-2010_06
专利号
US07732456B2

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