反応 #40935

反応方程式

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

Dess-Martin periodinane

Et2O

→

title compound

収率 68.0%

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

収率 68.0%

溶媒

THF

反応条件

後処理

1. 1
   洗浄the mixture washed with aqueous saturated NaHCO3 solution
2. 2
   乾燥The organic phase was dried (Na2SO4)
3. 3
   その他evaporated
4. 4
   その他The crude was purified by flash chromatography with ethyl acetate-petroleum ether (1-1)

実験手順

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).

出典