反応 #71996

反応方程式

cis(±)-4-Chloro-N-(3-ethoxypiperidin-4-yl)-5-ethyl-1H-imidazole-2-carboxamide hydrochloride

2-chloropyridine

sodium carbonate

→

title compound

収率 3.5%

cis(±)-4-Chloro-N-(3-ethoxy-1-pyridin-2-ylpiperidin-4-yl)-5-ethyl-1H-imidazole-2-carboxamide

収率 3.5%

溶媒

DMF

ethyl acetate

反応条件

後処理

1. 1
   温度the suspension was heated
2. 2
   その他at 180° C.
3. 3
   その他for 30 minutes
4. 4
   洗浄washed with water and brine
5. 5
   乾燥dried over anhydrous sodium sulfate
6. 6
   濃縮concentration under reduced pressure
7. 7
   その他the residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=7/3→1/0)

実験手順

cis(±)-4-Chloro-N-(3-ethoxypiperidin-4-yl)-5-ethyl-1H-imidazole-2-carboxamide hydrochloride obtained in Example (131a) (100 mg, 0.297 mmol), 2-chloropyridine (0.035 mL, 0.37 mmol) and sodium carbonate (157 mg, 1.48 mmol) were suspended in DMF (1 mL), and the suspension was heated using a microwave reactor at 180° C. for 30 minutes. The reaction solution was diluted with ethyl acetate, washed with water and brine, and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=7/3→1/0) to obtain 3.9 mg of the title compound as a white amorphous solid (3%).

出典