反応 #2069957
ord-0f3df3919ae94f048dc7b5f4ca7c0d04
反応方程式
反応物
試薬
なし
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度under reflux for 1 hour 30 minutes
- 2温度The mixture was cooled on ice
- 3抽出extracted with ethyl acetate
- 4乾燥dried over anhydrous magnesium sulfate
- 5濃縮concentrated under reduced pressure
- 6その他The residue was purified by silica gel column chromatography
実験手順
Phosphorus oxychloride (1.6 ml) was added to a solution of the compound of Example B145 (600 mg, 1.7 mmol) in acetonitrile (15 ml), and the mixture was stirred under reflux for 1 hour 30 minutes. The mixture was cooled on ice, made alkaline with a 5% aqueous sodium hydrogencarbonate solution, extracted with ethyl acetate, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (82 mg).