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

HRID 1275875

반응식

HRID 1275875 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-976ad2b4a1e644e5a95fa7b91b4f4051
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06162808

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