反応 #76770

ord-0f13797f74d449c092f060ea899a8952

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added dropwise at 5° C.
  2. 2
    workup.ADDITIONThe reaction mixture was poured onto ice
  3. 3
    ろ過the precipitated crystals were collected by filtration
  4. 4
    洗浄washed with water
  5. 5
    その他dried

実験手順

Then, 110 g (0.44 mol) of methyl 2-bromo-4-fluorophenoxyformate was dissolved in 250 ml of sulfuric acid, to which a mixed acid of 30 g of fuming nitric acid and 30 ml of sulfuric acid was added dropwise at 5° C. or lower, and the mixture was stirred for 2 hours. The reaction mixture was poured onto ice, and the precipitated crystals were collected by filtration, washed with water, and dried, which afforded 126 g (0.43 mol) of methyl 2-bromo-4-fluoro-5-nitrophenoxyformate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06703503B2uspto-grants-2004_03