反应详情

温度

-20 °C

5-Butylthiophene-2-sulfonic acid tert-butylamide (2.9 g, 0.010 mol, see step (a) above) was dissolved in THF (40 mL) under N2 and then cooled to −78° C. n-BuLi (1.6 M, 16.2 mL, 0.026 mol) was added via a syringe. The reaction mixture was stirred at −20° C. for 4 hours. Tri-iso-propylborate (13.3 mL, 0.058 mol) was then added via a syringe and the reaction mixture was stirred overnight at room temperature. The reaction was quenched with 2 M HCl (20 mL). The organic phase was separated and the water phase was extracted with EtOAc (3×100 mL). The combined organic phase was washed with brine and dried and concentrated in vacuo. The product was used in the next step without further purification.

1. additionwas added via a syringe
2. stirringthe reaction mixture was stirred overnight at room temperature
3. customThe reaction was quenched with 2 M HCl (20 mL)
4. customThe organic phase was separated
5. extractionthe water phase was extracted with EtOAc (3×100 mL)
6. washThe combined organic phase was washed with brine
7. customdried
8. concentrationconcentrated in vacuo
9. customThe product was used in the next step without further purification