反应详情

温度

150 °C

A mixture of 6-methoxy-1-phenoxyisoquinoline (21.3 g, 85 mmol) and ammonium acetate (55 g) was heated, under a nitrogen atmosphere, to 150° C. and stirred overnight. The mixture was allowed to cool to ambient temperature, after which 3 N sodium hydroxide (280 ml) was added with stirring. The thus obtained solution was extracted with ethyl acetate (2×300 ml) and the combined organic layers were extracted with 2N hydrochloric acid (100 ml). Subsequently, the pH of the aqueous layer was adjusted to 12 with 2 N sodium hydroxide. Extraction with ethyl acetate (300 ml) then afforded an organic layer, which was washed with brine (100 ml), dried (magnesium sulphate) and concentrated under reduced pressure to give 1-amino-6-methoxyisoquinoline (11 g, 75%), ESI-MS: 175.2 [M+H]+

1. temperatureto cool to ambient temperature
2. stirringwith stirring
3. extractionThe thus obtained solution was extracted with ethyl acetate (2×300 ml)
4. extractionthe combined organic layers were extracted with 2N hydrochloric acid (100 ml)
5. extractionExtraction with ethyl acetate (300 ml)
6. customthen afforded an organic layer, which
7. washwas washed with brine (100 ml)
8. dry with materialdried (magnesium sulphate)
9. concentrationconcentrated under reduced pressure