反应详情

A mixture of 15.7 g (100 mmol) of 2-chloro-3-formyl-4-aminopyridine [338452-92-9], 37.6 ml (300 mmol) of tert-butyl methyl ketone, 1.0 ml (10 mmol) of piperidine and 100 ml of ethanol is heated under reflux for 60 h. After cooling, the reaction mixture is diluted with 500 ml of dichloromethane, washed five times with 500 ml of water each time, dried over magnesium sulfate, and the solvent is removed in vacuo. The residue is recrystallised from ethanol. Yield: 8.2 g (37 mmol), 37%. Purity: >95% according to 1H-NMR.

1. temperatureis heated
2. temperatureunder reflux for 60 h
3. temperatureAfter cooling
4. washwashed five times with 500 ml of water each time
5. dry with materialdried over magnesium sulfate
6. customthe solvent is removed in vacuo
7. customThe residue is recrystallised from ethanol