Hydrochloric Acid → HCID 19385473, compound

Participants

Reaction Conditions

Reaction Steps

5.0 g (18 mmol) of 3-hydrazino-6-(4-difluoromethoxy-3-methoxyphenyl)pyridazine are dissolved in 50 ml of ethanol and 2.3 ml (27 mmol) of concentrated hydrochloric acid, 1 g of palladium/carbon and 3.4 g (54 mmol) of ammonium formate are added, and the mixture is heated to 80° C. After evolution of gases has ceased, the mixture is stirred for a further 3 hours, filtered to remove the catalyst, and the solution is stirred in 1 l water and made alkaline with concentrated ammonia, and the resulting precipitate is collected on a suction funnel. The filter cake is thoroughly washed with water and then dried and chromatographed in a 95:5 mixture of dichloromethane/methanol on silica gel. The appropriate fractions are concentrated in vacuo. 3 g (63.6%) of 3-amino-6-(4-difluoromethoxy-3-methoxyphenyl)pyridazine of m.p. 184° C. are obtained.

Provenance & Evidence