反応 #742984

ord-8d8961b4498f45c493c8ac48ba937f36

反応方程式

O=[N+]([O-])O
nitric acid
Cc1cccc(C)c1Br
2,6-dimethyl bromobenzene
Cc1ccc([N+](=O)[O-])c(C)c1Br
yellow solid
Cc1ccc([N+](=O)[O-])c(C)c1Br
2,6-Dimethyl-3-nitrobromo Benzene

溶媒

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled in an ice-bath (above f.p)
  2. 2
    その他to come to rt
  3. 3
    その他Reaction mixture
  4. 4
    温度was cooled
  5. 5
    ろ過The resulting yellow solid was filtered
  6. 6
    洗浄washed with ice-water
  7. 7
    その他dried

実験手順

Fuming nitric acid (83.3 mL) (>90%) was added slowly to a solution of 2,6-dimethyl bromobenzene (27.9 g, 150 mmol) in acetric acid (167 mL) and cooled in an ice-bath (above f.p). The mix was allowed to come to rt and later heated at 80° C. for 2 h. (HPLC showed no SM). Reaction mixture was cooled and poured into ice-water with stirring. The resulting yellow solid was filtered, washed with ice-water and dried to give 28.7 g of an yellow solid which was used as such in the next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08071609B2uspto-grants-2011_12