反応 #2501404

ord-677ec35014b0470caa8a41ef9c3e3026

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出The solution was extracted with ethyl acetate
  2. 2
    乾燥the combined extracts were dried over Na2SO4
  3. 3
    その他Removal of solvent

実験手順

4-Cyanoisophthalic acid dimethyl ester 203 (1.70 g, 7.76 mmol) was dissolved in methanol (100 mL) and then treated with an aqueous solution of lithium hydroxide (2.0 g, 46.5 mmol) in 50 mL of water. The basic solution was stirred at ambient temperature for 1.5 hour. It was then poured into a 10% HCl solution. The solution was extracted with ethyl acetate and the combined extracts were dried over Na2SO4. Removal of solvent gave quantitative yield of 4-cyanoisophthalic acid 204: 1H NMR (400 MHz, CD3OD) δ 8.01 (d, J=8 Hz, 1H), 8.33 (dd, J=1.7 Hz, J=8 Hz, 1H), 8.73 (d, J=1.7 Hz, 1H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06811979B2uspto-grants-2004_11