HRID1644823

反应详情

EQUATION

反应方程式

HRID 1644823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

5-iso-Butyl-N-tert-butylthiophene-2-sulfonamide (10.6 g, 0.039 mol, see step (b)) above) was dissolved in THF (165 mL) under N2 and then cooled to −78° C. n-BuLi (1.6 M, 60.19 mL, 0.096 mol) was added via a syringe. The reaction mixture was stirred at −20° C. for 4 h. The 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, dried and concentrated in vacuo. The product was used without further purification.

WORKUP

后处理

  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 without further purification