反应详情

To a solution of 3,6-dichloro-4-(1,1-dimethylethyl)pyridazine (2.0 g, 9.76 mmol) in ethanol (30 ml) was added hydrazine hydrate (0.34 ml, 10.9 mmol) dropwise. The reaction mixture was heated at reflux for 18 h under an atmosphere of nitrogen. The solvent was removed under high vacuum to leave a residue to which was added 5N hydrochloric acid (50 ml). The solution obtained was washed with dichloromethane (20 ml) and the aqueous layer was poured on to a mixture of ice and aqueous ammonia. The resultant solid was collected by filtration and dried under vacuum to yield the title compound (1.2 g). Data for the title compound: 1H NMR (360 MHz, DMSO) δ1.39 (3H, t, J=7.3 Hz), 4.35 (2H), 7.07 (1H, s), 8.07 (1H, s); MS (ES+) m/e 201, 203 [MH]+.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 18 h under an atmosphere of nitrogen
3. customThe solvent was removed under high vacuum
4. customto leave a residue to which
5. customThe solution obtained
6. washwas washed with dichloromethane (20 ml)
7. additionthe aqueous layer was poured on to a mixture of ice and aqueous ammonia
8. filtrationThe resultant solid was collected by filtration
9. customdried under vacuum