HRID2145

反应详情

EQUATION

反应方程式

HRID 2145 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-(3,4-dimethoxybenzenesulphonyl)-3-methoxycarbonyl-1,2,3,4-tetrahydro-isoquinoline(0.5 g) in THF (30 ml) was treated with a saturated aqueous solution of lithium hydroxide (3 ml) at room temperature. After stirring overnight, the solvent was removed in vacuo. The residue was diluted with water (10 ml), washed with ethyl acetate (10 ml) and acidified with 2M hydrochloric acid. The aqueous phase was extracted with ethyl acetate (2×30 ml); these extracts were combined and dried (magnesium sulphate). Evaporation of the solvent in vacuo and recrystallization of the residue from ethyl acetate/hexane afforded the title compound as a whim solid (0.44 g).

WORKUP

后处理

  1. customthe solvent was removed in vacuo
  2. additionThe residue was diluted with water (10 ml)
  3. washwashed with ethyl acetate (10 ml)
  4. extractionThe aqueous phase was extracted with ethyl acetate (2×30 ml)
  5. dry with materialdried (magnesium sulphate)
  6. customEvaporation of the solvent
  7. customin vacuo and recrystallization of the residue from ethyl acetate/hexane