反応 #10643

反応方程式

4-bromoisoquinoline

ammonia

→

title compound

4-aminoisoquinoline

溶媒

1,4-dioxane

反応条件

後処理

1. 1
   温度The reaction mixture was cooled to room temperature
2. 2
   その他the insoluble matters were removed by filtration through Celite
3. 3
   抽出the filtrate was extracted twice with ethyl acetate (150 ml for each time)
4. 4
   乾燥The organic layer was dried over anhydrous sodium sulfate
5. 5
   その他the solvent was evaporated under reduced pressure
6. 6
   その他The residue was purified by silica gel column chromatography (chloroform:methanol=9:1)

実験手順

A suspension of 4-bromoisoquinoline (25.0 g), copper(II) sulfate pentahydrate (30.4 g, Nacalai Tesque), 28% aqueous ammonia (100 ml) and 1,4-dioxane (100 ml) was stirred in a sealed tube at 165° C. for 21 hours. The reaction mixture was cooled to room temperature, the insoluble matters were removed by filtration through Celite, and the filtrate was extracted twice with ethyl acetate (150 ml for each time). The organic layer was dried over anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=9:1) to obtain the title compound (13.2 g).

出典