Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl piperazine-1-acetate | HCID 207112 | — |
| Reactant | 6-Chloro-5-nitropyridine-3-carboxylic acid | HCID 346459 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67342117 | HCID 67342117 | 162.2% |
Reaction Steps
A mixture of 2.00 g (9.87 mmol) of 6-chloro-5-nitro-nicotinic acid and 2.03 g (11.8 mmol) of piperazin-1-yl-acetic acid ethyl ester in N,N-dimethylformamide (10 mL) are heated to 130° C. in a microwave reactor for 1 hour. The resulting dark mixture is poured into water which forms a precipitate. The pH of the mixture is adjusted to approximately pH 2 by adding concentrated hydrochloric acid. The precipitated solid is collected by filtration, washed with water, and dried under reduced pressure to give 2.70 g (81.1%) of 4-ethoxycarbonylmethyl-3′-nitro-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-5′-carboxylic acid as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08952004B2 |
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| Source dataset | uspto-grants-2015_02 |
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| ORD ID | ord-f12f5119bee6499397c638662be3804e |
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| Source note | uspto-grants-2015_02 |
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