HRID1366754

反应详情

EQUATION

反应方程式

HRID 1366754 的结构方程式

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A mixture of the crude 6-methoxy-7-methyl-1-phenoxyisoquinoline (9 g, 33.96 mmol) and ammonium acetate (26 g) was melted with stirring at 170° C. for 5 h. The mixture was partitioned between aqueous sodium hydroxide (2 M) and ethyl acetate. The phases were separated and the organic phase extracted with dilute aqueous hydrochloric acid. The acidic aqueous phase was neutralized to pH 12 using sodium hydroxide (2M), extracted with ethyl acetate, dried (MgSO4) then dried in vacuo to give 6-methoxy-7-methylisoquinolin-1-ylamine (5.11 g, 27.18 mmol).

WORKUP

后处理

  1. customThe mixture was partitioned between aqueous sodium hydroxide (2 M) and ethyl acetate
  2. customThe phases were separated
  3. extractionthe organic phase extracted with dilute aqueous hydrochloric acid
  4. extractionextracted with ethyl acetate
  5. dry with materialdried (MgSO4)
  6. customthen dried in vacuo