HRID1499550

反应详情

EQUATION

反应方程式

HRID 1499550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of 1,3-difluoro-5-(methylthio)benzene (0.800 g, 4.99 mmol) in dry THF (25 mL) under nitrogen at −78° C., n-BuLi in THF (1.6 M; 3.28 mL, 5.24 mmol) was added slowly while keeping the internal temperature below −65° C. The reaction mixture was stirred at −78° C. for 2 h. 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (1.07 g, 5.74 mmol) was then added. The reaction mixture was allowed to warm to room temperature for 2 h, and then quenched with aq. NaHCO3 and extracted with EtOAc. The organic extracts were washed with brine, dried, filtered and concentrated under reduced pressure to yield the crude sub-title compound (1.42 g, 99%) as a viscous liquid.

WORKUP

后处理

  1. customthe internal temperature below −65° C
  2. temperatureto warm to room temperature for 2 h
  3. customquenched with aq. NaHCO3
  4. extractionextracted with EtOAc
  5. washThe organic extracts were washed with brine
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure