反应详情

A solution of 7.3 g (47 mmol) of 2-mercaptonicotinic acid and 9.6 g (48 mmol) of 2-(p-toluenesulfonyl)-ethanol was dissolved in DMF (80 ml). 0.5 ml of conc. H2SO4 was then carefully added dropwise, and stirring was carried out overnight under reflux. The reaction mixture was concentrated using a Genevac (EZ2). The residue was dissolved in acetonitrile and the solid was separated off. The mother liquor was concentrated, and MeOH was added. The resulting solid was filtered off and dried. 2.35 g (7 mmol, 14.8%) of 2-(2-tosylethylthio)nicotinic acid were obtained as solid.

1. temperatureunder reflux
2. concentrationThe reaction mixture was concentrated
3. dissolutionThe residue was dissolved in acetonitrile
4. customthe solid was separated off
5. concentrationThe mother liquor was concentrated
6. additionMeOH was added
7. filtrationThe resulting solid was filtered off
8. customdried