HRID1366754
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customThe mixture was partitioned between aqueous sodium hydroxide (2 M) and ethyl acetate
- customThe phases were separated
- extractionthe organic phase extracted with dilute aqueous hydrochloric acid
- extractionextracted with ethyl acetate
- dry with materialdried (MgSO4)
- customthen dried in vacuo