반응 #88236

ord-ebac018909a54f20af991c206b66b15b

반응 방정식

O=C([O-])[O-].[K+].[K+]
potassium carbonate
Cc1cc[nH]c(=O)c1[N+](=O)[O-]
4-methyl-3-nitropyridin-2(1H)-one
O=P(Br)(Br)Br
phosphorus oxybromide
Cc1ccnc(Br)c1[N+](=O)[O-]
title compound
수율 71.8%
Cc1ccnc(Br)c1[N+](=O)[O-]
2-bromo-4-methyl-3-nitropyridine
수율 71.8%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at the ambient temperature
  2. 2
    온도The reaction mixture was refluxed for 12 hours
  3. 3
    기타The organic layer was separated
  4. 4
    세척washed with water and brine
  5. 5
    건조dried over sodium sulfate
  6. 6
    기타The solvent was evaporated

실험 절차

The 4-methyl-3-nitropyridin-2(1H)-one (110 g, 0.71 mol) was suspended in dichloroethane (1 L). The solution of phosphorus oxybromide (317 g, 1.1 mol) in dichloroethane (1 L) was added dropwise thereto at the ambient temperature. The reaction mixture was refluxed for 12 hours. The mixture was allowed to cool to room temperature, poured into ice water, and neutralized with potassium carbonate. The organic layer was separated, washed with water and brine, and dried over sodium sulfate. The solvent was evaporated to provide the title compound (yield 71.8%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440968B2uspto-grants-2016_09