反应详情

A mixture of 2.70 g (7.40 mmol) of 6-(2,6-dichlorophenyl)-8-ethyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-ylideneamine of Example 65 and 15 mL of acetic anhydride was heated with stirring to the boiling point. The resulting solution was heated at reflux for 5 minutes and concentrated at reduced pressure to ca. 8 mL volume. The solution was cooled and ether (8 mL) was added. The well-defined crystals that separated were filtered and washed with 5 mL of ether and 10 mL of petroleum ether; wt 2.68 g; mp 175°-177° C.

1. temperaturewas heated
2. temperatureThe resulting solution was heated
3. temperatureat reflux for 5 minutes
4. concentrationconcentrated at reduced pressure to ca. 8 mL volume
5. temperatureThe solution was cooled
6. additionether (8 mL) was added
7. customThe well-defined crystals that separated
8. filtrationwere filtered
9. washwashed with 5 mL of ether and 10 mL of petroleum ether