反応 #501352
ord-6e1dfd46f81b43029b7b635cee379982
反応方程式
反応条件
後処理
- 1workup.ADDITIONA mixture of 106.5 gms
- 2workup.DISTILLATIONthe distillate collected
- 3その他for 30 minutes
- 4その他at 85° C.
- 5洗浄The top layer was washed with 50 gms
- 6その他water at 80°-85° C. and then separated
- 7その他stripped at 100°-105° C.
- 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##