反応 #3262
ord-040121136d37435a8bcc1f1ef88ef22c
反応方程式
反応条件
温度
25°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度was heated to reflux
- 2温度The resulting solution was maintained
- 3温度at reflux for 20 minutes
- 4濃縮concentrated at atmospheric pressure to about 0.25 mL volume
- 5workup.ADDITIONdiluted with diethyl ether (1 mL)
- 6ろ過The separated crystals were filtered
- 7洗浄washed with diethyl ether
実験手順
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.