반응 #161182

ord-372ad04aedf5491c98161c14d895b53e

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted twice with EtOAc
  2. 2
    세척The combined organic layers were washed with brine
  3. 3
    건조dried over MgSO4
  4. 4
    기타After removal of solvent
  5. 5
    기타the residue was purified by column chloromatography (0-5% EtOAc-Hexane)

실험 절차

To a mixture of 2-tert-butyl-4-bromo-5-nitrophenol (C-14-a) (1.1 g, 4 mmol) and Cs2CO3 (1.56 g, 4.8 mmol) in DMF (8 mL) was added benzyl bromide (500 μL, 4.2 mmol). The mixture was stirred at room temperature for 4 h, diluted with H2O and extracted twice with EtOAc. The combined organic layers were washed with brine and dried over MgSO4. After removal of solvent, the residue was purified by column chloromatography (0-5% EtOAc-Hexane) to yield 1-tert-butyl-2-(benzyloxy)-5-bromo-4-nitrobenzene (1.37 g, 94%). 1H NMR (400 MHz, CDCl3) 7.62 (s, 1H), 7.53 (s, 1H), 7.43 (m, 5H), 5.22 (s, 2H), 1.42 (s, 9H).

출처

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