反应详情

Ethyl acrylate (16.2 ml, 0.15 mol) and bis-(triphenylphosphine) palladium (II) chloride (0.84 g, 0.0012 mol) in DMF (75 ml) and Et3N (75 ml) was heated together at reflux under N2 with stirring until a homogeneous solution resulted. 2-[4-Bromo-5-(4-fluorophenyl))-3-(1-methylethyl)-1H-pyrazol-1-yl]pyrimidine (3) (10.8 g, 0.03 mol) was added and the resulting solution was heated at reflux for 24 hours, during which, an additional 1 mol % of catalyst was added. The mixture was then cooled to room temperature and diluted with ether and water. The organic layer was separated and washed with water and brine, dried over MgSO4, filtered and concentrated in vacuo. The resulting solid (10.4 g) was recrystallized from hexane/ethyl acetate, mp 155°-162° C.

1. temperatureat reflux under N2
2. customresulted
3. temperaturethe resulting solution was heated
4. temperatureat reflux for 24 hours, during which
5. additionan additional 1 mol % of catalyst was added
6. customThe organic layer was separated
7. washwashed with water and brine
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. customThe resulting solid (10.4 g) was recrystallized from hexane/ethyl acetate, mp 155°-162° C.