反応 #40972

反応方程式

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

収率 47.0%

溶媒

DMF

DMF

反応条件

後処理

1. 1
   workup.STIRRINGAfter stirring
2. 2
   その他the reaction at room temperature for 48 hours
3. 3
   抽出the mixture was extracted with diethylether
4. 4
   抽出The aqueous layer was then extracted with ethyl acetate
5. 5
   乾燥The organic phase was dried (Na2SO4)
6. 6
   ろ過filtered
7. 7
   その他evaporated
8. 8
   その他the crude was used without further purification in the next step (200 mg, 47% yield)

実験手順

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).

出典