반응 #2355152

ord-50c4afaac15044c1b271561fc1c9d394

반응 조건

온도
75°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to cool to room temperature
  2. 2
    workup.ADDITIONwas poured
  3. 3
    기타over crushed ice
  4. 4
    추출a product of 1,5-bis(trifluoroacetoxy)pentan-3-one was extracted with dichloromethane
  5. 5
    건조After drying with MgSO4
  6. 6
    여과filtering
  7. 7
    기타removal of the solvent

실험 절차

A mixture of 17.85 g of 1,5-dichloropentan-3-one, 92 mL of trifluoroacetic acid, and 34.55 g of sodium trifluoroacetate was stirred and heated at 75° C. for 64 hours. The mixture was allowed to cool to room temperature, was poured over crushed ice, and a product of 1,5-bis(trifluoroacetoxy)pentan-3-one was extracted with dichloromethane. After drying with MgSO4, filtering, and removal of the solvent, 24.4 g of crude 1,5-bis(trifluoroacetoxy)pentan-3-one product was obtained. Analysis of the 1,5-bis(trifluoroacetoxy)pentan-3-one showed 1HNMR (CDCl3, TMS ref.): 2.94 (t, 4H), 4.63 (t, 4H) ppm.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06325876B1uspto-grants-2001_12