Water → 5-Bromo-2,4-bis(1,1-dimethylethoxy)pyrimidine

HRID 324392

反応式

HRID 324392 の反応式
[CH3:1][C:2]([CH3:5])([O-:4])[CH3:3].[K+].[Br:7][C:8]1[C:9](Cl)=[N:10][C:11](Cl)=[N:12][CH:13]=1.[OH2:16]>O1CCCC1>[Br:7][C:8]1[C:9]([O:16][C:2]([CH3:5])([CH3:3])[CH3:1])=[N:10][C:11]([O:4][C:2]([CH3:5])([CH3:3])[CH3:1])=[N:12][CH:13]=1

参加物

5

反応物 3

HCID 962WaterHCID 2899735-Bromo-2,4-dichloropyrimidineHCID 23665647Potassium tert-butoxide

生成物 1

HCID 8188515-Bromo-2,4-bis(1,1-dimethylethoxy)pyrimidine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of potassium tert-butoxide (67.5 g) in tetrahydrofuran (500 ml) was added 5-bromo-2,4-dichloropyrimidine (55 g) (J. Am. Chem. Soc., 1934, 56, 134) in tetrahydrofuran (100 ml) dropwise. After 1.5 hours water (100 ml) was added carefully and the mixture extracted with ethyl acetate. The combined organic solution was washed with water, dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with isohexane containing 1% triethylamine.

後処理

  1. extractionthe mixture extracted with ethyl acetate
  2. washThe combined organic solution was washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated under reduced pressure
  5. customPurification
  6. washeluting with isohexane containing 1% triethylamine

出典と根拠

ORDレコード
ord-2fa5f3caf1ce486d911a5439d93c7e09
出典データセット
uspto-grants-2001_04
特許番号
US06218376B1

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