HRID482817

反应详情

EQUATION

反应方程式

HRID 482817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

315 g of said terephthalaldehydic acid chloride dissolved in 400 ml of toluene was dropped into an ice-cooled mixed solution of commercially available S(-)-2-methylbutanol (optically active amyl alcohol) and 230 g of pyridine, and heated under reflux for 2 hours. The reaction solution was cooled to room temperature and further cooled with ice, and acidified by adding 6N hydrochloric acid thereto to remove pyridine in the organic layer. The organic layer was then washed successively with water, 2N aqueous sodium hydroxide solution, and again with water. Toluene as a solvent was distilled off in vacuum, and the remaining reaction product was distilled in vacuum to obtain p-(2-methylbutoxycarbonyl)benzaldehyde (b.p. 118°-124° C./3.5 Torr).

WORKUP

后处理

  1. temperaturecooled
  2. temperatureheated
  3. temperatureunder reflux for 2 hours
  4. temperaturefurther cooled with ice
  5. customto remove pyridine in the organic layer
  6. washThe organic layer was then washed successively with water, 2N aqueous sodium hydroxide solution
  7. distillationToluene as a solvent was distilled off in vacuum
  8. customthe remaining reaction product
  9. distillationwas distilled in vacuum