HRID35223

反应详情

EQUATION

反应方程式

HRID 35223 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3,4-dihydro-6,7-dimethoxy-1-methylisoquinoline hydrochloride (58.4 g, 0.24 m) in 1 liter of methanol and 5% Pd/C (5 g) were combined under nitrogen in a pressure bottle and the mixture hydrogenated at 40 psi and ambient temperature on a Parr apparatus for 18 hr. The catalyst was removed by filtration and the solvent evaporated. The residue was dissolved in H2O (1 liter), basified to pH 11 with 50% NaOH and extracted with CHCl3 (3×300 ml). The extracts were dried over MgSO4 and evaporated to dryness (aspirator, then high vacuum) to give 1,2,3,4-tetrahydro-6,7-dimethoxy-1-methylisoquinoline, 35.2 g (70% yield).

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. customthe solvent evaporated
  3. dissolutionThe residue was dissolved in H2O (1 liter)
  4. extractionextracted with CHCl3 (3×300 ml)
  5. dry with materialThe extracts were dried over MgSO4
  6. customevaporated to dryness (aspirator