反应详情

温度

100 °C

Sodium metal (130 mmol, 3.1 g) was added to benzyl alcohol (75 mL) and gently warmed to 50° C. for 30 minutes until all the sodium metal had dissolved. To this was added a solution of 3,6-dichloropyridazine (135 mmol) in benzyl alcohol (75 mL). The reaction was heated at 100° C. for 24 h. Excess benzyl alcohol was evaporated and the residue was extracted with EtOAc (3×100 mL). The EtOAc extract was washed with H2O. The EtOAc layer was collected, dried, filtered and the filtrate was evaporated to yield 3-benzyloxy-6-chloro-pyridazine (90%, 26.7 g); mp 77° C.-78° C.

1. dissolutionhad dissolved
2. customExcess benzyl alcohol was evaporated
3. extractionthe residue was extracted with EtOAc (3×100 mL)
4. extractionThe EtOAc extract
5. washwas washed with H2O
6. customThe EtOAc layer was collected
7. customdried
8. filtrationfiltered
9. customthe filtrate was evaporated