Reaktion #3262

ord-040121136d37435a8bcc1f1ef88ef22c

Reaktionsbedingungen

Temperatur
25°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated to reflux
  2. 2
    TemperaturThe resulting solution was maintained
  3. 3
    Temperaturat reflux for 20 minutes
  4. 4
    Einengenconcentrated at atmospheric pressure to about 0.25 mL volume
  5. 5
    workup.ADDITIONdiluted with diethyl ether (1 mL)
  6. 6
    FiltrationThe separated crystals were filtered
  7. 7
    Waschenwashed 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05733914uspto-grants-1998_03