反应详情

Into a 50-mL three neck round-bottom flask, was placed a solution of methyl 5-cyano-2,4-dimethylbenzoate (compound 2.3, 900 mg, 4.28 mmol, 1.00 equiv, 90%) in methanol (20 mL). Hydrogen chloride gas was introduced by bubbling through the solution for 0.5 hr. The reaction mixture was then transferred into a 30-mL sealed tube and stirred overnight at room temperature. The mixture was concentrated under vacuum and the residue was diluted with ethyl acetate (30 mL) and extracted with water (10 mL). The aqueous was concentrated in vacuo to obtain the title compound as a white solid (200 mg, 15%).

1. customby bubbling through the solution for 0.5 hr
2. customsealed tube
3. concentrationThe mixture was concentrated under vacuum
4. additionthe residue was diluted with ethyl acetate (30 mL)
5. extractionextracted with water (10 mL)
6. concentrationThe aqueous was concentrated in vacuo