반응 #41026

반응 방정식

1-bromo-4-chloro-butane

3-Benzoyl-5-iodo-1H-pyrimidine-2,4-dione

K2CO3

Water

1-bromo-4-chloro-butane

→

title compound

수율 98.0%

3-Benzoyl-1-(4-chloro-butyl)-5-iodo-1H-pyrimidine-2,4-dione

수율 98.0%

용매

DMF

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   추출the mixture was extracted with ethyl ether
3. 3
   건조The organic phase was dried (Na2SO4)
4. 4
   여과filtered
5. 5
   기타evaporated
6. 6
   기타the crude was purified by flash chromatography with petroleum ether-ethyl acetate (7-3)

실험 절차

3-Benzoyl-5-iodo-1H-pyrimidine-2,4-dione (Prep128, 2.5 g, 7.3 mmol), K2CO3 (1 g, 7.3 mmol) and 1-bromo-4-chloro-butane (1.26 ml, 10.95 mmol) were suspended in dry DMF (10 ml). After stirring the reaction at room temperature overnight, further 1-bromo-4-chloro-butane (840 μl, 7.3 mmol) was added. Water was added and the mixture was extracted with ethyl ether. The organic phase was dried (Na2SO4), filtered and evaporated; the crude was purified by flash chromatography with petroleum ether-ethyl acetate (7-3) to give the title compound as a white solid (3 g, 98% yield).

출처