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CAS No. : | 39929-79-8 | MDL No. : | MFCD03092515 |
Formula : | C6H5N3O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HASUWNAFLUMMFI-UHFFFAOYSA-N |
M.W : | 151.12 | Pubchem ID : | 11819216 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92.1% | Urea (30 g) was added to a solution of sodium ethoxide prepared from sodium (22 g), and absolute ethanol (300 mL) previously cooled to 5-10 °C. The mixture was stirred for 5 min and was treated with ethyl 2-cyano-4, 4-diethoxybutanoate (110 g). The resulting mixture was allowed to warm with stirring. The sodium salt dissolved with the evolution of heat, and the temperature of the mixture was maintained at 80 °C overnight. The reaction mixture was cooled and poured into 300 mL of water, and the solution was concentrated in vacuo. Next, the residue was acidified with concentrated HCl to produce a white precipitate, which was collected by filtration, washed with water and dried on a funnel to provide compound 17a (66.8 g, yield: 92.1percent).1H-NMR (400MHz, DMSO-d6): delta11.44 (1H, s), 11.09 (1H, s), 10.47 (1H, s), 6.56 (1H, t, J= 2.4 Hz), 6.22 (1H, t, J= 2.4 Hz). ESI-MS calculated for (C6H5N3O2) [M+H]+, 152.0, found 152.1. |