反应详情

To a solution of 2-Chloro-5-(2-ethoxy-vinyl)-pyrimidin-4-ylamine (38.0 g, 0.19 mol) in ETOH (1000 ml) is added concentrated aqueous HCl (37%, 100 g, 1.00 mol) at rt. The reaction mixture is heated to reflux for 3 h and then evaporated to dryness under reduced pressure. Aqueous sodium carbonate solution (5%, 500 mL) is added to the residue, and the mixture is extracted with EtOAc (3×). The combined organic layers are dried over MgSO4, filtered, and concentrated under reduced pressure. The residue is recrystallized from hexane/ether (4/1, 250 ml) to give the title compound as an off-white solid.

1. temperatureThe reaction mixture is heated
2. temperatureto reflux for 3 h
3. customevaporated to dryness under reduced pressure
4. additionAqueous sodium carbonate solution (5%, 500 mL) is added to the residue
5. extractionthe mixture is extracted with EtOAc (3×)
6. dry with materialThe combined organic layers are dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe residue is recrystallized from hexane/ether (4/1, 250 ml)