反应详情

温度

70 °C

To a solution of methyl 2-[2-Methyl-4-(4-methylphenyl)-6,7-dihydro-5H-cyclopenta[4,5]thieno[2,3-b]pyridin-3-yl]-3-phenylpropanoate (0.159 g; 0.36 mmol) in methanol (3.6 mL) was added a solution of sodium hydroxide 10 N (0.36 ml) and the mixture was heated at 70° C. for 4 h. After cooling, the reaction mixture was concentrated under reduced pressure and the crude solid was suspended in ethyl acetate and the mixture was acidified with 1N HCl (pH˜2). The organic layer was washed with brine, dried over sodium sulphate, filtered and concentrated under reduced pressure. The residue was purified by preparative thin layer chromatography on silica using a mixture ethyl acetate/heptane (1/1)+0.5% acetic acid as eluent to afford 0.056 g (38%) of the title compound as a white solid.

1. temperatureAfter cooling
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. washThe organic layer was washed with brine
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by preparative thin layer chromatography on silica using a mixture ethyl acetate/heptane (1/1)+0.5% acetic acid as eluent