Reaction #3143753
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04981963
Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: A suspension of N,N'-diacetyloxamide (10 g, 0.058 mol) in ethyl alcohol (20 ml) is charged into a three-necked flask equipped with a reflux condenser, an inlet tube for nitrogen, a dropping funnel, and a magnetic stirrer. 98 % Pyridine (40 ml, 0.40 mol) is then dripped therein at 70° C., and after 40 minutes the complete solving of N,N'-diacetyloxamide in the reaction mixture is observed. The temperature is brought to 95° C. and kept at this value for 6.5 hours. Then water (60 ml) and chloroform (60 ml) are added to the reaction mixture and the organic phase is separated. Chloroform is distilled off and ethyl ether (30 ml) is added to precipitate the compound of the title. The precipitate is recovered by filtration and dried, thus affording the compound of the title (5.1 g, 0.023 mol, yield 39.2%) with m.p. 88°-90° C. is charged into a three-necked flask equipped with a reflux condenser, an inlet tube for nitrogen, a dropping funnel, and a magnetic stirrer is brought to 95° C. the organic phase is separated Chloroform is distilled off ethyl ether (30 ml) is added to precipitate the compound of the title The precipitate is recovered by filtration dried thus affording the compound of the title (5.1 g, 0.023 mol, yield 39.2%) with m.p. 88°-90° C.
Source ID: ord-4d3599b3c7bd4f6f9a9e39fb515ac711