反应详情

温度

50 °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-methoxypropanoate (0.124 g; 0.31 mmol) in methanol (3.1 mL) was added a solution of sodium hydroxide 10 N (0.31 ml) and the mixture was heated to 50° C. for 18 h. After cooling, the reaction mixture was carefully acidified with 1N HCl (pH˜2) and partially concentrated under reduced pressure. The residue was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over sodium sulphate, filtered and concentrated under reduced pressure. The residue was crystallized from a mixture of ethyl acetate/heptane to afford 0.038 g (32%) of the title compound as a beige powder.

1. temperatureAfter cooling
2. concentrationpartially concentrated under reduced pressure
3. customThe residue was partitioned between ethyl acetate and water
4. washThe organic layer was washed with brine
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was crystallized from a mixture of ethyl acetate/heptane