반응 #645362

반응 방정식

3-chloro-5,6-dihydrobenzo[h]cinnoline

1-(pyridin-2-yl)piperazine

ammonium hydrochloride

→

5,6-dihydro-3-(4-(pyridm-2-yl)piperazin-1-yl)benzo[h]cinnoline

수율 81.1%

용매

반응 조건

후처리

1. 1
   기타the solvent was removed under reduced pressure
2. 2
   추출The remaining residue was then extracted with ethyl acetate
3. 3
   세척washed with water and brine
4. 4
   건조dried over anhydrous Na2SO4
5. 5
   기타Removal of solvent
6. 6
   기타followed by recrystallization from 95% ethanol
7. 7
   기타yielded light yellow crystals, yield 81.1%

실험 절차

A mixture of comprising about 0.01 mol of 3-chloro-5,6-dihydrobenzo[h]cinnoline, about 0.05 mol of 1-(pyridin-2-yl)piperazine and about 0.01 mol of ammonium hydrochloride was prepared in about 15 ml of 1-BuOH. The mixture was stirred at 130° C. for 48 h, and then the solvent was removed under reduced pressure. The remaining residue was then extracted with ethyl acetate, washed with water and brine, dried over anhydrous Na2SO4. Removal of solvent followed by recrystallization from 95% ethanol yielded light yellow crystals, yield 81.1%; HPLC: 96.4% purity; HRMS calculated 343.1791, found 343.1787; 1H NMR (CDCl3): 5 8.452 (d, J=7.5, 1H), 8.232 (s, 1H), 7.211-7.534 (m, 4H), 6.794 (s, 1H), 6.678-6.731 (m, 2H), 3.862 (d, J=4.0, 4H), 3.745 (d, J=4.0, 4H), 2.918 (s, 4H).

출처