반응 #1135849

ord-0dd9dd478f49401db6ef76e7eed3cbed

반응 방정식

Nc1c(-c2cccnc2)cncc1[N+](=O)[O-]
5-nitro-3,3′-bipyridin-4-amine
Nc1cncc(-c2cccnc2)c1N
3,3′-bipyridine-4,5-diamine

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solution was purged with hydrogen
  2. 2
    여과The suspension was filtered through Celite
  3. 3
    농축the concentrated under vacuum

실험 절차

To a solution of 5-nitro-3,3′-bipyridin-4-amine (XIV) (5 g, 23 mmol) in MeOH (20 mL) was added 10% Pd/C. The solution was purged with hydrogen and stirred at r.t. under hydrogen for 15 h. The suspension was filtered through Celite and the concentrated under vacuum to produce 3,3′-bipyridine-4,5-diamine (XV) as off white solid (3.3 g, 17.7 mmol, 76% yield). 1H NMR (DMSO-d6, 400 MHz,): δ 8.63-8.53 (m, 1H), 7.90-7.83 (m, 1H), 7.75 (s, 1H), 7.58 (s, 1H), 7.48-7.43 (m, 2H), 6.13 (bs, 2H), 5.31 (bs, 2H). ESIMS found C10H10N4 m/z 187.10 (M+H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09381192B2uspto-grants-2016_07