反应详情

Concentrated HCl (25 mL) was added to N-tert-butyl-2-chloro-5-[(E)-2-ethoxyvinyl]pyrimidin-4-amine (5.3 g, 20.72 mmol) (see Preparation 61) in isopropanol (210 mL) and the mixture was heated at reflux for 4 hours. The reaction mixture was then evaporated in vacuo and the residue was basified with saturated aqueous NaHCO3 and extracted with EtOAc (200 mL). The organic extract was dried over sodium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel (gradient of hexane:EtOAc 93:7 to 90:10) to afford the title compound as a yellow oil in 85% yield, 3.7 g.

1. temperaturethe mixture was heated
2. temperatureat reflux for 4 hours
3. customThe reaction mixture was then evaporated in vacuo
4. extractionextracted with EtOAc (200 mL)
5. extractionThe organic extract
6. dry with materialwas dried over sodium sulfate
7. customevaporated in vacuo
8. customThe residue was purified by column chromatography on silica gel (gradient of hexane:EtOAc 93:7 to 90:10)