反应详情

To picolinamidine hydrochloride (1-1-g) (112 g, 0.71 mol) in MeOH (1.1 L) was added sodium methoxide (39.4 g, 0.71 mol) and diethyl ethoxymethylenemalonate (142 g, 0.71 mol). The reaction mixture was heated at reflux overnight and then cooled to room temperature. The resulting mixture was filtered and to the filtrate was added potassium hydroxide (71.4 g, 1.37 mol) in water (265 mL). The reaction was heated at reflux for 2 h. The reaction was cooled to room temperature before adding concentrated HCl (180 mL, 2.35 mol) in portions. The reaction was aged for 2 h. The solids were filtered and rinsed with EtOH, Et2O and then hexane to provide the product, 1-1-h, (110 g, 65%).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. filtrationThe resulting mixture was filtered and to the filtrate
4. temperatureThe reaction was heated
5. temperatureat reflux for 2 h
6. temperatureThe reaction was cooled to room temperature
7. filtrationThe solids were filtered
8. washrinsed with EtOH, Et2O
9. customhexane to provide the product, 1-1-h, (110 g, 65%)