Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | N-Iodosuccinimide | HCID 120273 | — |
| Reactant | ethyl 2-methyl-6-oxo-1,6-dihydropyridine-3-carboxylate | HCID 3299500 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58117243 | HCID 58117243 | — |
Reaction Steps
N-Iodosuccinimide (40 g, 180 mmol) was added to a suspension of intermediate (5b), 2-methyl-6-oxo-1,6-dihydro-pyridine-3-carboxylic acid ethyl ester (18.1 g, 100 mmol) in acetonitrile (400 mL), under a nitrogen atmosphere. The resulting suspension was heated at 95° C. for 5 hours to give an initial orange solution. An off-white precipitate slowly formed. The resulting suspension was allowed to cool and was poured into water (1200 mL) to give an off-white precipitate. The separated by filtration and the solids washed with water (500 mL) to give an off-white powder. The solids were dried in vacuo (60° C.) to give the product as an off-white powder, 28.3 g (92%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08916591B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-528ccf711f0e4a7caa3e0c18cc37e075 |
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| Source note | uspto-grants-2014_12 |
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