反应详情

A mixture of 4,6-dichloro-pyrimidin-2-yl-amine (6.6 g, 40 mmol), 4-aminobenzyl alcohol (8.0 g, 65 mmol) and N,N-diisopropylethylamine (15 ml) in ethanol (200 ml) was heated under reflux for 72 hours. Concentration under reduced pressure provided a solid which was stirred with 1.0 M hydrochloric acid (200 ml) for 1 hour, filtered, dried under reduced pressure, stirred with ethyl acetate (200 ml) for 2 hours, filtered, and dissolved in methanol (300 ml). Aqueous sodium carbonate solution (1.0 M, 50 ml) was added. After stirring for 2 hours, volatiles were evaporated under reduced pressure and water (200 ml) was added. Filtration and drying provided [4-(2-amino-6-chloro-pyrimidin-4-yl-amino)-phenyl]-methanol (6.3 g, 63% yield) as a white powder.

1. temperaturewas heated
2. temperatureunder reflux for 72 hours
3. concentrationConcentration under reduced pressure
4. customprovided a solid which
5. filtrationfiltered
6. customdried under reduced pressure
7. filtrationfiltered
8. dissolutiondissolved in methanol (300 ml)
9. additionAqueous sodium carbonate solution (1.0 M, 50 ml) was added
10. stirringAfter stirring for 2 hours
11. customvolatiles were evaporated under reduced pressure and water (200 ml)
12. additionwas added
13. filtrationFiltration
14. customdrying