HRID80534

反应详情

EQUATION

反应方程式

HRID 80534 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Chloro-3-fluorobenzaldehyde (2.5 g) and (R)-(+)-2-methyl-2-propanesulfinamide were dissolved in dichloromethane (50 ml), and then titanium(IV) isopropoxide (23.6 ml) was added. The mixture was heated for three hours under reflux, then poured onto ice (150 g) and stirred vigorously for ten minutes. The mixture was filtered through kieselguhr and the filtrate was extracted with dichloromethane (3×50 ml). The organic phase was dried (Na2SO4), filtered and concentrated under reduced pressure. The product (4 g) was used further without further purification.

WORKUP

后处理

  1. temperatureThe mixture was heated for three hours
  2. temperatureunder reflux
  3. additionpoured onto ice (150 g)
  4. filtrationThe mixture was filtered through kieselguhr
  5. extractionthe filtrate was extracted with dichloromethane (3×50 ml)
  6. dry with materialThe organic phase was dried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe product (4 g) was used further without further purification