反応 #1583817
ord-210e112c9e3943e5a593e0ca7177feb1
反応方程式
sulphuric acid
N-benzyl-4-[2-ethyl-4-(4-fluorophenyl)-1,3-thiazol-5-yl]pyridine-2-amine
sodium hydroxide
→
4-[2-Ethyl-4-(4-fluorophenyl)-1,3-thiazol-5-yl]pyridine-2-amine
反応物
試薬
なし
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1抽出the mixture is extracted with dichloromethane (3×100 ml)
- 2乾燥The combined organic phases are dried over MgSO4
- 3その他The residue is triturated with MTBE
- 4ろ過filtered off
- 5その他The product obtained
実験手順
With ice cooling, 23 ml of conc. sulphuric acid are added to 4.75 g (10.9 mmol) of N-benzyl-4-[2-ethyl-4-(4-fluorophenyl)-1,3-thiazol-5-yl]pyridine-2-amine, and the reaction mixture is stirred at room temperature for 30 min. The reaction mixture is stirred into 100 ml of ice-water, the pH is adjusted to 10 using concentrated aqueous sodium hydroxide solution and the mixture is extracted with dichloromethane (3×100 ml). The combined organic phases are dried over MgSO4 and freed from the solvent under reduced pressure. The residue is triturated with MTBE and filtered off. The product obtained is 2.80 g (82%) of a beige solid; log P (pH2.7): 1.29 with MS (ESI): 300.1 ([M+H]+).