反应 #61164

反应方程式

4-chloro-2-fluoronitrobenzene

piperidine

water

→

title compound

收率 97.0%

1-(5-Chloro-2-nitro-phenyl)-piperidine

收率 97.0%

溶剂

EtOH

反应条件

后处理

1. 1
   workup.WAITat 23° C. for 30 min
2. 2
   萃取extracted with EtOAc (2×30 mL)
3. 3
   洗涤The combined extracts were washed with saturated aq NaHCO3 and brine (30 mL each)
4. 4
   干燥dried (Na2SO4)
5. 5
   浓缩Concentration

实验过程

To a cooled (0° C.) solution of 1.75 g (10.0 mmol) of 4-chloro-2-fluoronitrobenzene in 15 mL of EtOH was added 2.97 mL (30.0 mmol) of piperidine dropwise over 5 min. The solution stirred at 0° C. for 10 min and then at 23° C. for 30 min. The mixture was poured into water (225 mL) and extracted with EtOAc (2×30 mL). The combined extracts were washed with saturated aq NaHCO3 and brine (30 mL each) and then dried (Na2SO4). Concentration afforded 2.33 g (97%) of the title compound as an orange oil which crystallized on standing: Mass spectrum (ESI, m/z): Calcd. for C11H13ClN2O2, 241.1 (M+H), found 241.1.

来源