反应详情

To a solution of KOH (0.18 g, 3.21 mmol) in 8.0 mL water and 3.0 mL methanol was added ethyl-3-methyl-4-hydroxy-5-tert-butyl-7-(2-thienoyl)-benzofuran-2-carboxylate, compound 13 (0.412 g, 1.07 mmol). The reaction mixture was heated to reflux for 0.5 hours. The resulting solution was cooled in an ice bath and acidified by the dropwise addition of 2N HCl. The acid was collected by filtration, washed with water and pulled dry over night on the filter funnel to give desired product sufficiently pure for further use. mp 145° C. with decarboxylation; 1H NMR (DMSO-d6) d 1.44 (9H, s), 2.76 (3H, s), 7.17 (1H, dd, J=4 Hz), 7.73 (2H, d, J=4 Hz), 7.90 (1H, s).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 0.5 hours
3. temperatureThe resulting solution was cooled in an ice bath
4. filtrationThe acid was collected by filtration
5. washwashed with water
6. custompulled dry over night on the filter funnel