HRID27163

反应详情

EQUATION

反应方程式

HRID 27163 的结构方程式

PROCEDURE

实验过程

To 1-(N-benzyloxycarbonyl-p-benzyloxyanilinomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline p-toluenesulfonate (10.0 g) was added a saturated sodium bicarbonate aqueous solution and then the mixture was extracted with ethyl acetate. The extract was washed with water, dried and the solvent was distilled off to give 1-(N-benzyloxycarbonyl-p-benzyloxyanilinomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline (8.2 g). To this residue (8.2 g) were added conc. hydrochloric acid (50 ml) and ethanol (50 ml) and the mixture was refluxed for 4 hours with stirring. The reaction mixture was concentrated to dryness under reduced pressure and the residue was pulverized with ether to give a powder of 1-(p-hydroxyanilinomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline dihydrochloride (5.8 g), mp 170° to 184° C. (dec).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. distillationthe solvent was distilled off