反応 #411516

反応方程式

4-piperidinone monohydrate hydrochloride

2,4-difluorobenzoyl chloride

→

product

収率 71.0%

4-(2,4-Difluorobenzoyl)piperidinone

収率 71.0%

溶媒

CH2Cl2

triethylamine

反応条件

後処理

1. 1
   その他before quenching with aqueous NaHCO3 (30 mL)
2. 2
   抽出Extracted with EtOAc (3×50 mL)
3. 3
   乾燥dried (MgSO4)
4. 4
   濃縮concentrated to a residue which
5. 5
   その他was purified by flash chromatography (EtOAc:Hexanes 9:1 to 1:1 )

実験手順

To a suspension of 4-piperidinone monohydrate hydrochloride (2.00 g, 13.28 mmol) in CH2Cl2 (40 mL) and triethylamine (5.0 mL) was added 2,4-difluorobenzoyl chloride (2.84 g, 15.93 mmol). The resulting mixture was stirred at room temperature for 5 hours before quenching with aqueous NaHCO3 (30 mL). Extracted with EtOAc (3×50 mL), dried (MgSO4), and concentrated to a residue which was purified by flash chromatography (EtOAc:Hexanes 9:1 to 1:1 ) afford product as an oil (2.25 g, 71%).

出典