反应详情

Dry HCl (gas) was bubbled through a MeOH (30 mL) solution of 2-cyanopyridine from Step 1 (1.4 g, 9.6 mmol) at 0° C. until saturation. The flask was sealed with a new rubber septum and the reaction mixture was stirred 30 hours at r.t. After careful depressurisation, H2O (5 mL) was added and the MeOH was evaporated. The aqueous residue was neutralized with saturated aq. NaHCO3 and extracted with EtOAc (3×). The organic extracts were dried over MgSO4, concentrated in vacuo, and the residue was purified by flash chromatography (from 30% to 50% EtOAc in hexanes) to give 1.49 g (87%) of the title compound.

1. customThe flask was sealed with a new rubber septum
2. customthe MeOH was evaporated
3. extractionextracted with EtOAc (3×)
4. dry with materialThe organic extracts were dried over MgSO4
5. concentrationconcentrated in vacuo
6. customthe residue was purified by flash chromatography (from 30% to 50% EtOAc in hexanes)