反応 #501352

ord-6e1dfd46f81b43029b7b635cee379982

反応方程式

CCCCCCCCCCCCCCCCCCCCCCO
behenyl alcohol
O=C(O)c1ccccc1
benzoic acid
CCCCCCCCCCCCCCCCCCCCCCOC(=O)c1ccccc1
Behenyl Benzoate

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONA mixture of 106.5 gms
  2. 2
    workup.DISTILLATIONthe distillate collected
  3. 3
    その他for 30 minutes
  4. 4
    その他at 85° C.
  5. 5
    洗浄The top layer was washed with 50 gms
  6. 6
    その他water at 80°-85° C. and then separated
  7. 7
    その他stripped at 100°-105° C.
  8. 8
    その他to remove residual moisture

実験手順

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##

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04791097uspto-grants-1988_12