HRID1608854

反应详情

EQUATION

反应方程式

HRID 1608854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20 g of 2-amino-5-bromo-2'-fluorobenzophenone are heated at 85° C. for 48 hours in 120 ml of dry pyridine in the presence of 20 g of 3,4-dimethoxyphenylsulfonyl chloride. The mixture is cooled, poured into ice-cold water, the solid is filtered off, the solid is extracted with AcOEt, the organic phase is washed with water, a solution of hydrochloric acid (1N), water and then saline water. After drying over magnesium sulfate and evaporating the solvent under vacuum, a solid is obtained which is recrystallized from DCM/isopropyl ether.

WORKUP

后处理

  1. temperatureThe mixture is cooled
  2. additionpoured into ice-cold water
  3. filtrationthe solid is filtered off
  4. extractionthe solid is extracted with AcOEt
  5. washthe organic phase is washed with water
  6. dry with materialAfter drying over magnesium sulfate
  7. customevaporating the solvent under vacuum
  8. customa solid is obtained which
  9. customis recrystallized from DCM/isopropyl ether