反应详情

A mixture of 3-chloro-6-methoxy pyridazine (0.69 mol, 100 g), thiourea (1.38 mol, 105 g) and ethyl methyl ketone (1.8 L) was refluxed for 3 hours. The reaction was cooled and the supernatant was poured into water and extracted with 1M sodium hydroxide (4×100 mL). The sodium hydroxide solution was washed with EtOAc (2×50 mL), the aqueous extract was acidified with sufficient conc. HCl to lower the pH to 5 and the resulting yellow solid was collected and air-dried to obtain 3-mercapto-6-methoxy pyridazine (24%, 23 g); mp 198° C.-200° C.

1. temperaturewas refluxed for 3 hours
2. temperatureThe reaction was cooled
3. extractionextracted with 1M sodium hydroxide (4×100 mL)
4. washThe sodium hydroxide solution was washed with EtOAc (2×50 mL)
5. extractionthe aqueous extract
6. customthe resulting yellow solid was collected
7. customair-dried