反应详情

温度

135 °C

To a solution of 6.3 g (0.023 mol) of 3-(2-quinazolinylmethoxy)benzenacetonitrile in 150 ml of dimethylformamide are added 7.5 g (0.115 mol) of sodium azide and 6.2 g (0.115 mol) of ammonium chloride, and the slurry is heated to 135° C. for 72 hours. The slurry is poured into 500 ml of water/500 ml of ethyl acetate, and the layers are separated. The aqueous phase is twice extracted with 250 ml of ethyl acetate, and the combined ethyl acetate solution is twice washed with 500 ml of water, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain 4 g of crystals, m.p. 129°-131° C. Recrystallization from ethanol gives 2.5 g (34%) of crystals, m.p. 129°-131° C., MS(CI) 319 (M+H).

1. customthe layers are separated
2. extractionThe aqueous phase is twice extracted with 250 ml of ethyl acetate
3. washthe combined ethyl acetate solution is twice washed with 500 ml of water
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated in vacuo