反应 #3247694
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04780542
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 1.722 g. (0.01 mole) of decanoic acid and 1.5 ml triethylamine in 25 ml water was prepared by warming on a water bath. The solution was rapidly cooled in an ice-salt bath while stirring. After the temperature of about -2° C. was reached, 1.0 ml. ethyl chloroformate was slowly added along with about 2 g. of crushed ice. Stirring was continuted for an additional hour (internal temperature was maintained) between 0 and -2° C.). Finally 1.5 ml. benzyl alcohol was added. Stirring of the reaction mixture was continued for 1/2 hour on a 60° water bath. After cooling, the ester was extracted twice by 30 ml ether, washed with sodium, bicarbonate solution then with water. After drying and evaporation of the solvent, the ester was distilled under reduced pressure to give 2.574 g. (99% yield) of benzyldecanoate. B.P. 208-210/15 mm. Anal. Calcd. for C17H26O2 :c, 77.82; H, 9.98. Found: C, 77.69; H, 10.03. by warming on a water bath The solution was rapidly cooled in an ice-salt bath After the temperature of about -2° C. Stirring was continuted for an additional hour (internal temperature was maintained) between 0 and -2° C.) Stirring of the reaction mixture After cooling the ester was extracted twice by 30 ml ether washed with sodium, bicarbonate solution After drying evaporation of the solvent the ester was distilled under reduced pressure to give 2.574 g
来源 ID: ord-3b9e6a5f0a2842ce8b3a71762b0bdf01