تفاعل #40937

معادلة التفاعل

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

Dess-Martin periodinane

Et2O

→

title compound

المردود 51.7%

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

المردود 51.7%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   غسيلthe solution washed with aqueous saturated NaHCO3
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-(4-Hydroxy-butyl)-5-trifluoromethyl-1H-pyrimidine-2,4-dione (Prep 23, 44 mg, 0.17 mmol) was dissolved in dry THF (5 mL), the solution was cooled to 0° C. and Dess-Martin periodinane (127 mg, 0.28 mmol) was added. The mixture was stirred at 0° C. for 1.5 hours. Et2O was added and the solution washed with aqueous saturated NaHCO3. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography with ethyl acetate-petroleum ether (1-1) to give 22 mg of the title compound (50% yield).

المصدر