반응 #161192

ord-2f65493029c44c919174f8c8a75f400c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture was filtered
  2. 2
    농축the filtrate was concentrated
  3. 3
    기타The crude product was recrystallized from ethyl acetate and petroleum ether

실험 절차

To a solution of 2-tert-butyl-4-bromo-5-nitrophenol (C-14-a) (12 g, 43.8 mmol) in MeOH (90 mL) was added Ni (2.4 g). The reaction mixture was stirred under H2 (1 atm) for 4 h. The mixture was filtered and the filtrate was concentrated. The crude product was recrystallized from ethyl acetate and petroleum ether to give 2-tert-butyl-4-bromo-5-amino-phenol (C-27) (7.2 g, 70%). 1H NMR (DMSO-d6) δ 9.15 (s, 1H), 6.91 (s, 1H), 6.24 (s, 1H), 4.90 (br s, 2H), 1.22 (s, 9H); ESI-MS 244.0 m/z (MH+).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08829204B2uspto-grants-2014_09