反应详情

A solution of 3.0 g (17.6 mmol) 6-chloro-N-methyl-nicotinamide in 42.0 ml THF was treated at 4° C. dropwise over 15 min. with 43.8 ml (43.8 mmol) o-tolylmagnesiumchloride-solution (IM in THF). The reaction mixture was stirred for 2 h at r.t., cooled to 0° C. and treated dropwise with 50 ml 5% aqueous NH4Cl. The aqueous phase was separated and extracted twice with toluene and the organic phases were washed twice with 5% aqueous NH4Cl. The combined organic phases were dried over Na2SO4 and the solvent was removed under reduced pressure to yield 5.4 g (94.6%) product as yellowish crystals, m.p. 137.0-138.0° C.

1. temperaturecooled to 0° C.
2. customThe aqueous phase was separated
3. extractionextracted twice with toluene
4. washthe organic phases were washed twice with 5% aqueous NH4Cl
5. dry with materialThe combined organic phases were dried over Na2SO4
6. customthe solvent was removed under reduced pressure