HRID920895

反应详情

EQUATION

反应方程式

HRID 920895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

A suspension of 24.97 g (57.3 mmol) of (bromomethyl)triphenylphosphonium bromide in 160 mL of THF was chilled to −70° C. under argon. Then, 6.43 g (57.3 mmol) of potassium tert-butoxide were added portionwise and the suspension was allowed to stir at this temperature for 1 h. A solution of 7.5 g of (47.7 mmol) quinoline-2-carbaldehyde in 40 mL of THF was slowly added dropwise. The mixture was allowed to stir at −75° C. for further 5 hours and then warmed to room temperature overnight. 160 mL of PE were added. The precipitate formed was sucked off. The mother liquid was evaporated and the residue was stirred with diisopropyl ether. The residue formed was sucked off. Purification by chromatography (heptane/EA 3/1) yielded 6.6 g (59.1%) of the title compound.

WORKUP

后处理

  1. stirringto stir at −75° C. for further 5 hours
  2. temperaturewarmed to room temperature overnight
  3. addition160 mL of PE were added
  4. customThe precipitate formed
  5. customThe mother liquid was evaporated
  6. stirringthe residue was stirred with diisopropyl ether
  7. customThe residue formed
  8. customPurification by chromatography (heptane/EA 3/1)