HRID870039

反应详情

EQUATION

反应方程式

HRID 870039 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

3,4-Dibromothiophene (15.5 g, 64.1 mmol) was added dropwise to a solution of n-BuLi (2.5M in hexane, 25.6 mL, 64.1 mmol) in Et2O (50 mL) at −78° C. After 1.5 h, 3-chlorobenzaldehyde (7.29 mL, 64.1 mmol) was added dropwise to the beige suspension. The resulting solution was stirred at −78° C. for 1 h and allowed to warm to 0° C. After 1 h, the reaction was quenched by the addition of 25% aq. NH4OAc. The aqueous layer was extracted with EtOAc and the combined organics were washed with water and brine, dried (Na2SO4) and concentrated to afford the desired product as a pale yellow oil. The crude product was used directly without further purification.

WORKUP

后处理

  1. temperatureto warm to 0° C
  2. waitAfter 1 h
  3. customthe reaction was quenched by the addition of 25% aq. NH4OAc
  4. extractionThe aqueous layer was extracted with EtOAc
  5. washthe combined organics were washed with water and brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated