Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | N,N'-Diacetyloxamide | HCID 3016168 | — |
| Product | HCID 12832643 | HCID 12832643 | 39.2% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04981963 |
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| Source dataset | uspto-grants-1991_01 |
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| ORD ID | ord-4d3599b3c7bd4f6f9a9e39fb515ac711 |
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| Source note | uspto-grants-1991_01 |
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