HRID1072507

反应详情

EQUATION

反应方程式

HRID 1072507 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.45 g (14.0 mmol) of 1-(4-bromo-phenyl)-2-[(2,4-dichloro-benzyl)-methyl-amino]-ethanol was introduced into 15 ml of dichloromethane and, at 0° C., 15 ml of conc. H2SO4 are added. After stirring at room temperature for 2 hours, the reaction mixture was poured onto ice and made alkaline with 6 N NaOH. Three extractions with dichloromethane were carried out. The combined organic phases were dried with MgSO4 and concentrated. For further purification, the residue was chromatographed on silica gel, resulting in 2.6 g of the title compound as a yellowish oil. 4-(4-Bromo-phenyl)-6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinoline, Hydrochloride;

WORKUP

后处理

  1. additionthe reaction mixture was poured onto ice
  2. extractionThree extractions with dichloromethane
  3. dry with materialThe combined organic phases were dried with MgSO4
  4. concentrationconcentrated
  5. customFor further purification
  6. customthe residue was chromatographed on silica gel