HRID1388808

反应详情

EQUATION

反应方程式

HRID 1388808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

67 ml of a 1.5 M solution of a mixed magnesium chloride complex of α-bromopropionic acid in THF was slowly added to 67 ml of a 1.5 M solution cooled to 10° C. of p-isobutylphenyl magnesium bromide in THF at such a rate that the temperature of the mixture was maintained at not more than 55° C. The resulting slurry was stirred at 50° C. for 1 hour, and then heated under reflux to allow about 50% of THF to distill. The reaction mixture was cooled, and diethyl ether and dilute hydrochloric acid were added. The organic layer was washed with water, dried, concentrated, and purified by silica gel column chromatography to give 4.4 g (yield 21.3%) of α-(p-isobutylphenyl)propionic acid.

WORKUP

后处理

  1. temperaturewas maintained at not more than 55° C
  2. temperatureheated
  3. temperatureunder reflux
  4. distillationto distill
  5. temperatureThe reaction mixture was cooled
  6. additiondiethyl ether and dilute hydrochloric acid were added
  7. washThe organic layer was washed with water
  8. customdried
  9. concentrationconcentrated
  10. custompurified by silica gel column chromatography