反応 #78102

ord-ad39031bca424b2097b7b12bee955401

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他at 0-5° C
  2. 2
    workup.ADDITIONAt the end of the addition the mixture
  3. 3
    ろ過The precipitate was filtered off
  4. 4
    洗浄washed thoroughly with water
  5. 5
    その他dried with suction

実験手順

A suspension of 4-fluorophenylacetic acid (10.0 g, 64.9 mmol) in concentrated sulfuric acid (100 ml) was cooled to 0° C. Concentrated nitric acid (4.5 ml, 65 mmol) was added drop-wise, keeping the temperature at 0-5° C. At the end of the addition the mixture was poured into ice-water (400 ml). The precipitate was filtered off, washed thoroughly with water and dried with suction to yield 1i (9.11 g, 70%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06710044B2uspto-grants-2004_03