反応 #1455185

ord-98286fbc60fe45f7bb46eb552012fb32

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The resulting solid was filtered
  2. 2
    洗浄washed

実験手順

To a solution of 4-trifluoromethylphenyl acetic acid (2.5 g, 12.25 mmol) in 8 mL of glacial acetic acid at 0° C. under an anhydrous atmosphere was added 5 mL of fuming H2SO4 (11% SO3) (caution!) followed by cautious addition of 90% HNO3 (3.5 mL, 73.14 mmol) within 10 min. The reaction mixture was then stirred at room temperature for 2 h and poured into ice-water. The resulting solid was filtered and washed with cold deionized water to give the desired product after drying as off-white solid, 2.5 g (82%); 1H NMR (200 MHz, CDCl3) δ 4.02 (s, 2H), 7.41 (d, J=8.0 Hz, 2H), 7.74 (d, J=8.0 Hz, 2H), 8.28 (s, 1H). The product was used directly into the following reactions.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE038133E1uspto-grants-2003_06