反应详情

790 mg of zinc powder are added to a mixture of 300 mg of 3-chloro-6-(4-fluorophenyl)[1,2,4]triazolo[4,3-b]pyridazine in 10 cm3 of glacial acetic acid at 20° C. After stirring for 1 h, the suspension is filtered and the filtrate is concentrated to dryness under vacuum. The oily residue is purified by dry deposit on Biotage Quad 12M (KP-SIL, 60 Å; 32-63 μm), elution being carried out with a 95:5 mixture of dichloromethane/methanol. 263 mg of 3-chloro-6-(4-fluorophenyl)-7,8-dihydro[1,2,4]triazolo[4,3-b]pyridazine are thus obtained in the form of a yellowy-brown powder, the characteristics of which are as follows:

1. filtrationthe suspension is filtered
2. concentrationthe filtrate is concentrated to dryness under vacuum
3. customThe oily residue is purified
4. customby dry deposit
5. washon Biotage Quad 12M (KP-SIL, 60 Å; 32-63 μm), elution
6. additionbeing carried out with a 95:5 mixture of dichloromethane/methanol