反応 #40944

反応方程式

1-(4-Hydroxy-butyl)-5-(3-methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione

Dess-Martin periodinane

Ethyl acetate

→

title compound

収率 98.0%

4-[5-(3-Methyl-thiophen-2-yl)-2,4-dioxo-3,4-dihydro-2H-pyrimidin-1-yl]-butyraldehyde

収率 98.0%

溶媒

DCM

反応条件

後処理

1. 1
   洗浄the solution washed with aqueous saturated Na2S2O3 (3 mL) and NaHCO3 (3 mL)
2. 2
   乾燥The organic phase was dried (Na2SO4)
3. 3
   その他evaporated

実験手順

1-(4-Hydroxy-butyl)-5-(3-methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione (Prep 31, 30 mg, 0.11 mmol) was dissolved in dry DCM (2 mL), the solution was cooled to 0° C. and Dess-Martin periodinane (113 mg, 0.26 mmol) was added portionwise under nitrogen. The mixture was stirred at room temperature for 1.5 hours. Ethyl acetate was added and the solution washed with aqueous saturated Na2S2O3 (3 mL) and NaHCO3 (3 mL). The organic phase was dried (Na2SO4) and evaporated to give 30 mg of the title compound that was used in the next step without further purification (98% yield).

出典