反应详情

A mixture of 10 g of nicotinic acid (0.08 mol), 25 g of thionyl chloride (0.21 mol), 1.5 ml of dimethylformamide and 200 ml of benzene was refluxed in an eggplant type flask for 3 hours. The solvent was removed by distillation. To the residue were added 20.8 g (0.16 mol) of 2-ethylhexyl alcohol and benzene, and the mixture was refluxed for 4 hours. The reaction mixture was poured into a saturated aqueous solution of sodium bicarbonate. The benzene layer was separated, washed successively with a saturated sodium bicarbonate aqueous solution, water and a saturated sodium chloride aqueous solution, dried over sodium sulfate and distilled to remove the solvent. The residue was purified by distillation under reduced pressure and column chromatography to obtain 9.1 g (70%) of 2-ethylhexyl nicotinate.

1. temperaturewas refluxed in an eggplant type flask for 3 hours
2. customThe solvent was removed by distillation
3. temperaturethe mixture was refluxed for 4 hours
4. customThe benzene layer was separated
5. washwashed successively with a saturated sodium bicarbonate aqueous solution, water
6. dry with materiala saturated sodium chloride aqueous solution, dried over sodium sulfate
7. distillationdistilled
8. customto remove the solvent
9. distillationThe residue was purified by distillation under reduced pressure and column chromatography