反应详情

温度

110 °C

A mixture of 2-chloro-6-methyl-5-nitronicotinonitrile (997 mg, 5.05 mmol), N-(cyclopentylmethy)-N-ethylamine (770 mg, 6.05 mmol), and K2CO3 (1.7 g, 12.3 mmol) in toluene (20 mL) is heated to 110° C. After stirring for 3 hours, the reaction mixture is filtered to remove the resulting precipitate. The filtrate is diluted with EtOAc and washed with H2O and brine. The organic layer is dried over sodium sulfate and concentrated in vacuo. The residue is purified by silica-gel column chromatography to give 2-[N-(cyclopentylmethyl)-N-ethylamino]-6-methyl-5-nitronicotinonitrile as orange oil.

1. filtrationthe reaction mixture is filtered
2. customto remove the resulting precipitate
3. additionThe filtrate is diluted with EtOAc
4. washwashed with H2O and brine
5. dry with materialThe organic layer is dried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue is purified by silica-gel column chromatography