反应详情

A mixture of 3-benzyloxy-6-chloro-pyridazine (18.2 mmol, 4 g), thiourea (36.3 mmol, 2.8 g) and ethyl methyl ketone (75 mL) was refluxed overnight. Excess ethyl methyl ketone was evaporated, the residue was extracted with 2M sodium hydroxide (25 mL) and the sodium hydroxide solution was washed with EtOAc (2×30 mL). The aqueous layer was collected and sufficient conc. HCl was added to bring the pH to 5 and extracted with EtOAc (2×30 mL). The EtOAc extract was collected, dried, filtered and the filtrate was evaporated to yield 3-benzyloxy-6-mercapto-pyridazine (15%, 605 mg); mp 155° C.-157° C.

1. temperaturewas refluxed overnight
2. customExcess ethyl methyl ketone was evaporated
3. extractionthe residue was extracted with 2M sodium hydroxide (25 mL)
4. washthe sodium hydroxide solution was washed with EtOAc (2×30 mL)
5. customThe aqueous layer was collected
6. additionsufficient conc. HCl was added
7. extractionextracted with EtOAc (2×30 mL)
8. extractionThe EtOAc extract
9. customwas collected
10. customdried
11. filtrationfiltered
12. customthe filtrate was evaporated