反应详情

A solution of 6-ethyl-nicotinonitrile (synthesis described in WO2008/71404, 1000 mg, 7.57 mmol), N-bromosuccinimide (1632 mg, 9.08 mmol) and 2,2′-azo-bis(isobutyronitrile) (62 mg, 0.38 mmol) in chloroform (12 mL) is heated at reflux for 7 min. After cooling to room temperature, the reaction mixture is filtered and the volatiles are removed under reduced pressure (260 mbar, 55° C.) to yield the product which was used without further purification. Yield: 1597 mg (quant.); ESI mass spectrum: [M+H]+=211 (Br pattern); Retention time HPLC: 0.92 min (Z018_S04).

1. temperatureat reflux for 7 min
2. filtrationthe reaction mixture is filtered
3. customthe volatiles are removed under reduced pressure (260 mbar, 55° C.)
4. customto yield the product which
5. customwas used without further purification
6. custom0.92 min (Z018_S04)