反应详情

A solution of n-butyl 6-[N-(5-bromo-2-hydroxybenzyl)-N-ethylamino]pyridazine-3-carboxylate (reference example 3) (0.286 g, 0.69 mmol) in DMF (3.5 ml) was treated with bromomethylcyclopropane (0.1 g, 0.78 mmol) and potassium carbonate (0.473 g, 3.4 mmol). The reaction was allowed to stir at ambient temperature for 60 hours. The solvent was evaporated at reduced pressure (vacuum pump) and the residue partitioned between ethyl acetate and water. The aqueous layer was extracted with ethyl acetate (2×10 ml). The organic layers were combined dried (MgSO4) and evaporated. The residue was purified by chromatography (eluant: ethyl acetate/hexane) to give the title compound as a pale yellow oil (0.3 g, 94%).

1. customThe solvent was evaporated at reduced pressure (vacuum pump)
2. customthe residue partitioned between ethyl acetate and water
3. extractionThe aqueous layer was extracted with ethyl acetate (2×10 ml)
4. dry with materialThe organic layers were combined dried (MgSO4)
5. customevaporated
6. customThe residue was purified by chromatography (eluant: ethyl acetate/hexane)