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

HRID 1275875

反応式

HRID 1275875 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 5% triethylamine in isohexane to give the product as a solid. Yield 52.4 g

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 5% triethylamine in isohexane

出典と根拠

ORDレコード
ord-976ad2b4a1e644e5a95fa7b91b4f4051
出典データセット
uspto-grants-2000_12
特許番号
US06162808

関連ノート

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