반응 #40972

반응 방정식

water

K2CO3

5-(2,4-Dimethyl-oxazol-5-yl)-1H-pyrimidine-2,4-dione

1-bromo-4-chloro-butane

→

1-(4-Chloro-butyl)-5-(2,4-dimethyl-oxazol-5-yl)-1H-pyrimidine-2,4-dione

수율 47.0%

용매

DMF

DMF

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring
2. 2
   기타the reaction at room temperature for 48 hours
3. 3
   추출the mixture was extracted with diethylether
4. 4
   추출The aqueous layer was then extracted with ethyl acetate
5. 5
   건조The organic phase was dried (Na2SO4)
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타the crude was used without further purification in the next step (200 mg, 47% yield)

실험 절차

5-(2,4-Dimethyl-oxazol-5-yl)-1H-pyrimidine-2,4-dione (Prep61, 300 mg, 1.45 mmol) was dissolved in dry DMF (4 ml) and K2CO3 (300 mg, 2.17 mmol) was added. The mixture was stirred at room temperature for 1 h, then a solution of 1-bromo-4-chloro-butane (commercially available from Aldrich, 496 mg, 2.9 mmol) in dry DMF (1 ml) was added. After stirring the reaction at room temperature for 48 hours, water was added and the mixture was extracted with diethylether. The aqueous layer was then extracted with ethyl acetate. The organic phase was dried (Na2SO4), filtered and evaporated; the crude was used without further purification in the next step (200 mg, 47% yield).

출처