反応 #81902
ord-26a020e1e80a4d4c857431a3c9c2b02f
反応方程式
反応物
試薬
なし
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.; MS (CI) 363 (M+ +1).