反应 #1481123
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05336663
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 31 ml of 100% nitric acid (dl.52) are introduced into the reaction vessel, and 6 g of o-chloropropiophenone are added dropwise at -10° C. in the course of 15 minutes in such a way that the reaction temperature is between -5° C. and -10° C. To complete the reaction, stirring is continued at 0° C. for 45 minutes. The reaction mixture is subsequently poured onto 300 g of ice, and the aqueous mixture is extracted twice using 200 ml portions of diethyl ether. The organic phase is washed with 100 ml of water, twice with 100 ml portions of 2N potassium hydrogen carbonate solution and finally with saturated sodium chloride solution, dried over magnesium sulfate and concentrated. The residue is recrystallised from diisopropyl ether/n-hexane; m.p.: 55°-56° C. are added dropwise at -10° C. in the course of 15 minutes in such a way that the reaction temperature is between -5° C. and -10° C the reaction the aqueous mixture is extracted twice The organic phase is washed with 100 ml of water, twice with 100 ml portions of 2N potassium hydrogen carbonate solution and finally with saturated sodium chloride solution dried over magnesium sulfate concentrated The residue is recrystallised from diisopropyl ether/n-hexane
来源 ID: ord-c0e6df6452fd40618555c238c2bd036e