反应详情

温度

150 °C

A mixture of 2-Amino-5-bromo-3-methylpyridine (15.49 g, 82.8 mmol) and Cu(I)CN (9.27 g, 103.5 mmol) in DMF (160 mL) was heated at 150° C. for 24 h. The reaction mixture was poured onto water and the solid which formed was extracted by using ethylacetate (600 mL, 3 times) from aq. NH4OH. The solvent was evaporated and the precipitate purified by chromatography (SiO2, hexanes/EtOAc 4:6). Yield 70%, mp 198-200° C., (Lit. mp 203-205° C.; see Dunn A. D. and Norrie R. J. Prakt. Chem./Chem.-Ztg, 338 (7), 663-666 (1996). Lit. melting point not reported via palladium-catalyzed cyanation; see Maligres, P. et al., Tetrahedron Lett., 40, 8193-8195 (1999).

1. additionThe reaction mixture was poured onto water
2. customthe solid which formed
3. extractionwas extracted
4. customThe solvent was evaporated
5. customthe precipitate purified by chromatography (SiO2, hexanes/EtOAc 4:6)