反应详情

To a stirred solution of copper (I) cyanide (18.31 g) in dry THF (400 ml) was added, at −78 C, tertbutylmagnesium chloride (1M in THF, 409 ml). The reaction mixture was stirred at this temperature for 15 min before slowly adding a solution of 2-bromo-5-[(phenylmethyl)oxy]pyridine (13.5 g) in THF. This was stirred for 2 h at −78 C before warming to 25-30 C and stirring for a further 20 h. The reaction mixture was poured into water and extracted with ethyl acetate. This was concentrated in vacuo and purified through silica, eluting with 0-2% ethyl acetate in hexane. Appropriate fractions were combined and concentrated in vacuo to yield the title compound, 6.3 g

1. stirringThis was stirred for 2 h at −78 C
2. temperaturebefore warming to 25-30 C
3. stirringstirring for a further 20 h
4. extractionextracted with ethyl acetate
5. concentrationThis was concentrated in vacuo
6. custompurified through silica
7. washeluting with 0-2% ethyl acetate in hexane
8. concentrationconcentrated in vacuo