反应详情

To ethyl 6-(trifluoromethyl)-1-benzothiophene-2-carboxylate dissolved in THF and MeOH was added a solution of LiOH in H2O (1.5 equiv). The reaction media became cloudy so H2O, MeOH and THF were added until a clear solution ensued (Final composition of media=2 THF:1 MeOH:1 H2O) (0.2 M). After 1 h, analysis showed consumption of all the starting material. A large proportion of the volatiles were removed under reduced pressure. The remaining solution was treated with 1N HCl. The precipitate was filtered off and dissolved in a mixture of THF, MeOH and EtOAc. The organic solution was dried over magnesium sulfate and concentrated under reduced pressure to obtain the title compound as a solid. The latter was ground with a mortar and pestle and let dry overnight under high vacuum.

1. customThe reaction media
2. additionwere added until a clear solution
3. customconsumption of all the starting material
4. customA large proportion of the volatiles were removed under reduced pressure
5. additionThe remaining solution was treated with 1N HCl
6. filtrationThe precipitate was filtered off
7. dissolutiondissolved in a mixture of THF, MeOH and EtOAc
8. dry with materialThe organic solution was dried over magnesium sulfate
9. concentrationconcentrated under reduced pressure