반응 #501352

ord-6e1dfd46f81b43029b7b635cee379982

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONA mixture of 106.5 gms
  2. 2
    workup.DISTILLATIONthe distillate collected
  3. 3
    기타for 30 minutes
  4. 4
    기타at 85° C.
  5. 5
    세척The top layer was washed with 50 gms
  6. 6
    기타water at 80°-85° C. and then separated
  7. 7
    기타stripped at 100°-105° C.
  8. 8
    기타to remove residual moisture

실험 절차

A mixture of 106.5 gms. (0.326 moles) of behenyl alcohol, 43.5 gms. (0.343 moles) of benzoic acid and 225 mgms. stannous oxalate was heated to 230° C. under nitrogen. The reaction was held at 230° C. for two hours, and the distillate collected. It was then cooled to 100° C. The acidity was 10.0 mg KOH/gm. The ester was then given a treatment for 30 minutes at 85° C. with 50 gms. deionized water, 2 gms. sodium carbonate, 2 gms. sodium chloride, and 1 gm. hydrogen peroxide. It was then allowed to stand and the lower aqueous layer drained off. The top layer was washed with 50 gms. water at 80°-85° C. and then separated. The solid was then vacuum stripped at 100°-105° C. to remove residual moisture. The final product was a solid benzoate ester having the following formula: ##STR14##

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04791097uspto-grants-1988_12