反应详情

温度

100 °C

a mixture of 756 mg of commercial 3,6-dichloro[1,2,4]triazolo[4,3-b]pyridazine, 0.352 cm3 of 2-hydroxymethyloxetane and 552 mg of potassium carbonate in 8 cm3 of N,N-dimethylformamide is heated at 100° C. for 6 h and then stirred at 20° C. overnight. The reaction medium is concentrated to dryness under vacuum. The residue obtained is purified by chromatography on a Merck cartridge of 25 g of silica 15-40 μm by solid deposit, elution being carried out with a dichloromethane/methanol gradient of 100/0 to 97/03. 701 mg of 3-chloro-6-(oxetan-2-ylmethoxy)[1,2,4]triazolo[4,3-b]pyridazine are thus obtained in the form of a beige solid, the characteristics of which are as follows:

1. concentrationThe reaction medium is concentrated to dryness under vacuum
2. customThe residue obtained
3. customis purified by chromatography on a Merck cartridge of 25 g of silica 15-40 μm by solid deposit, elution