Ethanol → HCID 58045983, compound

Participants

Reaction Conditions

Reaction Steps

6-Chloro-8-trifluoromethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine (W2.004; 65 mg) was initially charged in ethanol (6 ml) and admixed with sodium ethoxide (21 mg). The reaction mixture was stirred at 50° C. for 4 h. After cooling, the mixture was admixed with water and concentrated. The residue was taken up in ethyl acetate and washed with water three times. The ethyl acetate phase was dried over sodium sulfate, filtered and concentrated. The crude product was purified by means of preparative HPLC (met. E). The product-containing fractions, each of them clean, were combined, freed of the acetonitrile, adjusted to pH 9 with sodium hydrogencarbonate and extracted three times with ethyl acetate. The combined organic extracts were dried over sodium carbonate, filtered and concentrated. 15 mg of 6-ethoxy-8-trifluoromethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine and 23 mg of 6-ethoxy-8-(ethoxydifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine were obtained.

Provenance & Evidence