反应详情

温度

120 °C

A round-bottomed flask was charged with 3,5-dibromobenzonitrile (15.65 g, 60.00 mmol), sodium azide (7.80 g, 120.00 mmol) and zinc bromide (27.00 g, 120.00 mmol). After degassed, DMF (100 mL) was added. The reaction mixture was heated to 120° C. and stirred at this temperature until complete. The reaction was cooled to rt and then in an ice-water bath. 300 mL of 1N aqueous HCl was added. The white precipitate formed was collected by suction filtration, washed with water, and dried together with phosphorous pentoxide under vacuum to afford 17.32 g (95%) of product.

1. customAfter degassed
2. additionDMF (100 mL) was added
3. temperatureThe reaction was cooled to rt
4. addition300 mL of 1N aqueous HCl was added
5. customThe white precipitate formed
6. filtrationwas collected by suction filtration
7. washwashed with water
8. dry with materialdried together with phosphorous pentoxide under vacuum