反应详情

温度

110 °C

6-[N-(5-Bromo-2-propoxybenzyl)-N-ethylamino]-3-cyanopyridazine (reference example 18) (1.0 g, 2.67 mmol), was dissolved in DMA (15 ml) and treated with sodium azide (520 mg, 8.0 mmol) followed by triethylammonium chloride (550 mg, 4.0 mmol) and the mixture heated at 110° C. for 3 hours. The solution was poured 2M hydrochloric acid (50 ml), extracted with ethyl acetate and dichloromethane (100 ml of each) and the combined extracts washed with water (3×100 ml), dried over MgSO4 and concentrated in vacuo. Addition of ether and hexane precipitated a solid which was triturated with acetonitrile/toluene to give the title compound (965mg, 87%).

1. extractionextracted with ethyl acetate and dichloromethane (100 ml of each) and the combined extracts
2. washwashed with water (3×100 ml)
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo
5. additionAddition of ether and hexane
6. customprecipitated a solid which
7. customwas triturated with acetonitrile/toluene