반응 #54741

ord-b2e501a44b29474a8101c5558508fdb5

반응 방정식

O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
CC(C)Cc1ccc(CC(=O)O)cc1
p-isobutylphenylacetic acid
O=S(=O)(O)O
sulfuric acid
OCC(F)(F)F
2,2,2-trifluoroethanol
CC(C)Cc1ccc(CC(=O)OCC(F)(F)F)cc1
p-isobutylphenylacetic acid-2,2,2-trifluoroethyl ester

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 5 hours
  2. 2
    추출extracted with ether
  3. 3
    기타The ether layer separated
  4. 4
    농축concentrated
  5. 5
    기타to leave an oily residue
  6. 6
    workup.DISTILLATIONThe residue was distilled in vacuo

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04150137uspto-grants-1979_04