反応 #2898

ord-ac7f5eb35ef547d1a557dea38319f19e

反応方程式

CI
iodomethane
Cc1n[nH]c(C)c1Br
4-Bromo-3,5-dimethylpyrazole
[H-].[Na+]
sodium hydride
O=C([O-])O.[Na+]
sodium hydrogen carbonate
[H][H]
hydrogen
Cc1nn(C)c(C)c1Br
title compound
Cc1nn(C)c(C)c1Br
4-Bromo-1,3,5-trimethylpyrazole

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    その他evaporation under high vacuum
  3. 3
    その他the residue was purified by column chromatography

実験手順

4-Bromo-3,5-dimethylpyrazole (10 g) in dry dimethylformamide (50 ml) was added to a stirred suspension of sodium hydride (1.8 g) in dry dimethylformamide at 0° C. When the evolution of hydrogen was complete, iodomethane (8.9 g) was added dropwise. The mixture was allowed to warm to room temperature and after 30 minutes saturated aqueous sodium hydrogen carbonate (5 ml) was added. Following evaporation under high vacuum, the residue was purified by column chromatography to give the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05731335uspto-grants-1998_03