反应 #70246

反应方程式

2,6-difluorobenzaldehyde

4-methanesulfonylpiperidine hydrochloride

DIPEA

→

2-fluoro-6-(4-methanesulfonylpiperidine-1-yl)benzaldehyde

收率 84.0%

溶剂

acetonitrile

反应条件

后处理

1. 1
   其他The mixture was evaporated
2. 2
   萃取extracted with dichloromethane and citric acid solution
3. 3
   洗涤The organic layer was washed with brine
4. 4
   干燥dried over sodium sulfate
5. 5
   其他evaporated
6. 6
   其他The crude solid was triturated with cold ethyl acetate

实验过程

In a 250 mL round bottom flask, 2,6-difluorobenzaldehyde (7.12 g, 5.4 mL, 50.1 mmol), 4-methanesulfonylpiperidine hydrochloride (10 g, 50.1 mmol) and DIPEA (7.77 g, 60.1 mmol) were combined with acetonitrile (75 mL). The mixture was stirred and heated at 80° C. overnight. The mixture was evaporated and extracted with dichloromethane and citric acid solution. The organic layer was washed with brine, dried over sodium sulfate, and evaporated. The crude solid was triturated with cold ethyl acetate to afford 2-fluoro-6-(4-methanesulfonylpiperidine-1-yl)benzaldehyde (12 g, 84% yield). LC-MS calcd for C13H16FNO3S (m/e) 285.08, obsd 286.0 (M+H).

来源