反応 #54741

ord-b2e501a44b29474a8101c5558508fdb5

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was refluxed for 5 hours
  2. 2
    抽出extracted with ether
  3. 3
    その他The ether layer separated
  4. 4
    濃縮concentrated
  5. 5
    その他to leave an oily residue
  6. 6
    workup.DISTILLATIONThe residue was distilled in vacuo

実験手順

A mixture of 1.9 g of p-isobutylphenylacetic acid, 10 ml of 2,2,2-trifluoroethanol and 1 ml of concentrated sulfuric acid was refluxed for 5 hours. After the reaction was complete, the mixture was poured into ice-water. The resulting mixture was neutralized with adding 5% sodium carbonate solution, and then extracted with ether. The ether layer separated was dehydrated and concentrated to leave an oily residue. The residue was distilled in vacuo to yield 2.3 g of p-isobutylphenylacetic acid-2,2,2-trifluoroethyl ester as a colorless liquid, boiling at 78°-79° C./1 mmHg. Analysis-Calculated for C14H17F3O2 : C, 61.30; H, 6.25. Found: C, 61.01; H, 6.15. Mass spectrum: parent ion 274 m/e.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04150137uspto-grants-1979_04