Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | 2,5-Dichloropyridine-3-carboxylic acid | HCID 2736085 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 29888498 | HCID 29888498 | 92% |
Reaction Steps
A mixture of 2,5-dichloronicotinic acid (1.76 g, 9.17 mmol), 41% aq. methylamine solution (7 mL), and 1,4-dioxane (6 mL) was heated at 160° C. under microwave irradiation for 20 min. After cooling, volatile material was distilled off, and the residue was dissolved in water (30 mL) and acidified to pH 3 by addition of 37% aq. hydrochloric acid solution. The precipitate was collected by filtration and triturated in DCM to produce the title compound (1.60 g, 92%). Off-white solid, MS (ISP): 187.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07678818B2 |
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| Source dataset | uspto-grants-2010_03 |
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| ORD ID | ord-4acd24e1d6bc4973a8e19c5771fed078 |
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| Source note | uspto-grants-2010_03 |
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