تفاعل #10643

معادلة التفاعل

4-bromoisoquinoline

ammonia

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title compound

4-aminoisoquinoline

المذيبات

1,4-dioxane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر