39870-05-8

289-95-2

75-07-0

39870-05-8

Example 1: General procedure for the synthesis of 4-pyrimidine acetophenone from pyrimidine and acetaldehyde 1. dissolve pyrimidine (2.5 g, 31.2 mmol) and acetaldehyde (10.8 mL, 192 mmol) in dichloromethane (190 mL) at 0 °C with stirring and slowly add 3.4 M sulfuric acid (15.6 mL). 2. The reaction solution was cooled to -5°C and the following two solutions were added dropwise through two different dropping funnels simultaneously over a period of about 30 minutes: - 80% tert-butyl hydroperoxide in tert-butyl oxide/water solution (23.4 mL) - A solution of ferrous sulfate heptahydrate (52.2 g) dissolved in 100 mL of water. 3. After the dropwise addition was completed, the reaction mixture was continued to be stirred at 0 °C for 2.5 hours. 4. After completion of the reaction, the phases were separated and the aqueous phase was extracted with dichloromethane (2 x 150 mL). 5. The organic phases were combined and washed sequentially with 10% aqueous sodium iodide, 10% aqueous Na2S2O5 and brine, then dried with anhydrous Na2SO4. 6. The dried organic phase was concentrated and the yellow solid obtained was absorbed with petroleum ether and filtered. 7. After drying, 4-pyrimidine ethanone was obtained as a brown solid (0.87 g, 23% yield).