تفاعل #40935

معادلة التفاعل

1-(3-Hydroxy-propyl)-5-trifluoromethyl-1H-pyrimidine-2,4-dione

Dess-Martin periodinane

Et2O

→

title compound

المردود 68.0%

3-(5-Trifluoromethyl-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-yl)-propionaldehyde

المردود 68.0%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   غسيلthe mixture washed with aqueous saturated NaHCO3 solution
2. 2
   تجفيفThe organic phase was dried (Na2SO4)
3. 3
   أخرىevaporated
4. 4
   أخرىThe crude was purified by flash chromatography with ethyl acetate-petroleum ether (1-1)

الإجراء التجريبي

1-(3-Hydroxy-propyl)-5-trifluoromethyl-1H-pyrimidine-2,4-dione (Prep20, 100 mg, 0.42 mmol) was dissolved in dry THF (5 mL), the solution was then cooled to 0° C. and Dess-Martin periodinane (300 mg, 0.71 mmol) was added. The mixture was stirred at 0° C. for 1.5 hours. Et2O was added and the mixture washed with aqueous saturated NaHCO3 solution. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography with ethyl acetate-petroleum ether (1-1) to give 50 mg of title compound (68% yield).

المصدر