反応 #53550

ord-be524cb8b1a6445599b71a2c69566762

反応方程式

O=[N+]([O-])O
nitric acid
Cc1cccc(C)c1Br
2-bromo-m-xylene
Cc1ccc([N+](=O)[O-])c(C)c1Br
2,6-dimethyl-3-nitrobromobenzene

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled in an ice bath (above freezing point)
  2. 2
    温度heated at 80° C. for 2 hours or until the reaction
  3. 3
    温度The reaction mixture is cooled to room temperature
  4. 4
    workup.STIRRINGwith stirring
  5. 5
    その他The resulting yellow precipitates
  6. 6
    ろ過are collected by suction filtration and air
  7. 7
    その他dried

実験手順

Fuming nitric acid (>90% yellow fuming HNO3) is slowly added to a solution of 2-bromo-m-xylene (20 g, 150 mmol) in acetic acid (100 ml) cooled in an ice bath (above freezing point). The resulting mixture is allowed to warm to room temperature, stirred for 1 hour, and heated at 80° C. for 2 hours or until the reaction is shown to be complete by GC/MS analysis following micro-scale base work-up. The reaction mixture is cooled to room temperature and poured into ice/water with stirring. The resulting yellow precipitates are collected by suction filtration and air dried to obtain 2,6-dimethyl-3-nitrobromobenzene.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06858637B2uspto-grants-2005_02