反応 #1862533

反応方程式

ethyl piperidine-4-carboxylate

2-Bromo-4-methylpyridine

ethyl piperidine-4-carboxylate

DIPEA

→

brown solid

収率 56.0%

Ethyl 1-(4-methyl-2-pyridyl)piperidine-4-carboxylate

収率 56.0%

溶媒

dipropyleneglycolmonomethylether

反応条件

後処理

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITwas continued at 150° C. for 24 hours
3. 3
   濃縮The mixture was concentrated under reduced pressure
4. 4
   その他the residue was purified by column chromatography (silica, gradient from 0 to 30% ethyl acetate in DCM)

実験手順

2-Bromo-4-methylpyridine (860 mg, 5 mmol), ethyl piperidine-4-carboxylate (865 mg, 5.5 mmol) and DIPEA (958 μl, 5.5 mmol) were mixed in dipropyleneglycolmonomethylether (10 ml) and stirred at 150° C. overnight. Additional ethyl piperidine-4-carboxylate (865 mg, 5.5 mmol) was added and stirring was continued at 150° C. for 24 hours. The mixture was concentrated under reduced pressure and the residue was purified by column chromatography (silica, gradient from 0 to 30% ethyl acetate in DCM) to give 700 mg of a brown solid (2.8 mmol, 56%) MS (multi-mode) m/z=249.1 [M+1]+.

出典