反应详情

To a solution of methyl 2-(2,3,6-trimethyl-4-p-tolylthieno[2,3-b]pyridin-5-yl)pentanoate (0.074 g; 0.194 mmol) in methanol (4 mL) and ethanol (2 mL) was added a 5% sodium hydroxide solution (2 mL; 2.50 mmol). The reaction mixture was heated under reflux for 2 h. 5% sodium hydroxide solution (2 mL; 2.500 mmol) was added again and reflux was maintained for 2 h. 5% Sodium hydroxide solution (1 mL; 1.250 mmol) was added. After 3 h at reflux, 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 0.037 g (52%) of the title compound as a white powder.

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