反応 #51290

ord-7bb6164c432d43b09f578c4a6cbee1cc

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONpoured into a separatory funnel
  2. 2
    抽出The mixture was extracted into water
  3. 3
    洗浄washed with ether
  4. 4
    抽出extracted with ethyl acetate
  5. 5
    洗浄The organic layer was then washed with water and brine
  6. 6
    乾燥The organic layer was dried over sodium sulfate
  7. 7
    ろ過filtered
  8. 8
    濃縮concentrated under reduced pressure

実験手順

To a solution of methyl 2-azido-2-(3,5-difluorophenyl)acetate in THF/H2O (2.6:1) cooled to 0° C. was added 1.7 eq. of lithium hydroxide. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separatory funnel. The mixture was extracted into water and washed with ether. The aqueous layer was acidified with 1N HCl and extracted with ethyl acetate. The organic layer was then washed with water and brine. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to give 2-azido-2-(3,5-difluorophenyl)acetic acid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06849650B2uspto-grants-2005_02