반응 #54739

ord-8c1a8cb85b514d158b26466e15a975ed

반응 방정식

CC(C)Cc1ccc(CC#N)cc1
4-isobutylphenylacetonitrile
OCC(F)(F)F
2,2,2-trifluoroethanol
O=S(=O)(O)O
sulfuric acid
CC(C)Cc1ccc(CC(=O)OCC(F)(F)F)cc1
4-isobutylphenylacetic acid-2,2,2-trifluoroethyl ester
수율 51.1%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도were refluxed for 12 hours
  2. 2
    추출The resulting mixture was extracted 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 1.73 g of 4-isobutylphenylacetonitrile and 10 g of 95% of 2,2,2-trifluoroethanol and 10 g of concentrated sulfuric acid were refluxed for 12 hours. After the reaction was complete, ice-water was added to the mixture. The resulting mixture was extracted with ether. The ether layer separated was dehydrated and concentrated to leave an oily residue. The residue was distilled in vacuo to give 1.4 g of 4-isobutylphenylacetic acid-2,2,2-trifluoroethyl ester as a pale yellow oil, boiling at 77°-79° C./1 mmHg. Analysis-Calculated for C14H17F3O2 : C, 61.30; H, 6.25. Found: C, 61.21; H, 6.23.

출처

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