반응 #427497
ord-cd32b35f70fc4736998861954f9e4359
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과The insoluble solid was filtered off through celite
- 2농축the filtrate was concentrated en vacuo
- 3기타to obtain a crude residue
- 4세척The crude material was washed with 10% MeOH/DCM and 70% EtOAc/Hexanes
실험 절차
A mixture of 8-nitrobenzo[f][1,7]naphthyridin-5-amine (from the previous step) (1.0 eq) and Raney Nickel (wet, 10% wt) in EtOH/ammonia (2:1) was stirred under H2 balloon overnight. The reaction mixture was diluted with DCM. The insoluble solid was filtered off through celite, and the filtrate was concentrated en vacuo to obtain a crude residue. The crude material was washed with 10% MeOH/DCM and 70% EtOAc/Hexanes to give benzo[f][1,7]naphthyridine-5,8-diamine as an off white solid: 1H NMR (methanol-d4): δ 8.97 (dd, 1H), 8.90 (dd, 1H), 8.41 (d, 1H), 7.83 (dd, 1H), 7.57 (d, 1H), 7.39 (dd, 1H), 3.96 (s, 2). LRMS [M+H]=229.1.