Reaktion #3262
ord-040121136d37435a8bcc1f1ef88ef22c
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
25°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas heated to reflux
- 2TemperaturThe resulting solution was maintained
- 3Temperaturat reflux for 20 minutes
- 4Einengenconcentrated at atmospheric pressure to about 0.25 mL volume
- 5workup.ADDITIONdiluted with diethyl ether (1 mL)
- 6FiltrationThe separated crystals were filtered
- 7Waschenwashed with diethyl ether
Vorschrift
A mixture of 64.2 mg (0.20 mmol) of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7(8H)-one (from Example 12) and 1 mL of acetic anhydride was heated to reflux. The resulting solution was maintained at reflux for 20 minutes and concentrated at atmospheric pressure to about 0.25 mL volume. The solution was cooled to 25° C. and diluted with diethyl ether (1 mL). The separated crystals were filtered and washed with diethyl ether to provide N-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl]acetamide, wt 44.0 mg; mp 258°-260° C.