反应详情

To picolinamidine hydrochloride (10-b) (112 g, 0.71 mol) in MeOH (1.1 L) was added sodium methoxide (39.4 g, 0.71 mol) and diethyl ethoxymethylenemalonate (2-b) (142 g, 0.71 mol). The reaction 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 mixture was cooled to room temperature before adding conc. HCl (37%, 180 mL, 2.35 mol) in portions. The reaction aged for 2 h. The solids were filtered and rinsed with EtOH, Et2O and then hexane to provide compound 10-c (110 g, 65%).

1. temperatureThe reaction 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 mixture was cooled to room temperature
7. customThe reaction aged for 2 h
8. filtrationThe solids were filtered
9. washrinsed with EtOH, Et2O