반응 #4974

ord-1d5819da44804bb79114f5102ded9ad5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at 5° C.
  2. 2
    기타After the insoluble component was removed
  3. 3
    추출the solution was extracted with 100 ml of chloroform
  4. 4
    세척washed with saturated brine
  5. 5
    건조dried with Glauber's salt
  6. 6
    기타After removing Glauber's salt
  7. 7
    농축the solution was concentrated under reduced pressure
  8. 8
    기타the residue was recrystallized from hot hexane

실험 절차

87 ml of water and 18.2 ml (0.218 mol) of 12N-HCl were added to the solution of 87 ml of chloroform and 8.65 g (0.0121 mol) of the white solid containing 3,5-dihexadecyloxycarbonylbenzenesulfonyl chloride, and then 7.93 g of zinc was added thereto at 5° C. followed by stirring for 4 hours and 30 minutes. After the insoluble component was removed therefrom, the solution was extracted with 100 ml of chloroform, washed with saturated brine, and dried with Glauber's salt. After removing Glauber's salt, the solution was concentrated under reduced pressure, and the residue was recrystallized from hot hexane to obtain a colorless crystal of 3,5-dihexadecyloxycarbonylbenzenesulfonic acid. (Yield: 4.43 g, 48% (based on sodium 3,5-dimethyloxycarbonylbenzenesulfonate), m.p.: 63°-65° C.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05242785uspto-grants-1993_09