反应详情

To a solution of methyl 2-(2-ethyl-3,6-dimethyl-4-p-tolylthieno[2,3-b]pyridin-5-yl)pentanoate (0.119 g; 0.301 mmol) in methanol (6.4 mL) and ethanol (3.2 mL) was added a 5% sodium hydroxide solution (8.2 mL; 10.25 mmol). The reaction mixture was heated under reflux for 5.5 h. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. The residue was suspended in water, acidified with 1N HCl (pH˜2) and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over sodium sulphate, filtered and concentrated under reduced pressure. The residue was crystallized from a mixture of ethyl acetate/heptane to afford 0.059 g (51%) of the title compound as a white powder.

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux for 5.5 h
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with water and brine
6. dry with materialdried over sodium sulphate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe residue was crystallized from a mixture of ethyl acetate/heptane