HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 59028388, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2,6-Dichloroisonicotinic acid | HCID 94830 | — |
| Reactant | 2712421-24-2 | HCID 67249831 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59028388 | HCID 59028388 | 90.6% |
Reaction Steps
A solution of 2,6-dichloroisonicotinic acid (0.25 g, 1.3 mmol), methyl-[(methylcyclopropyl)methyl]amine hydrochloride (0.53 g, 3.9 mmol) and cesium carbonate (1.25 g, 6.5 mmol) in 5 mL DMF was heated to 120° C. in a sealed tube for 72 hr. The reaction was partitioned between 1M HCl and ethyl acetate. The organics were washed with water (4×), brine, dried over sodium sulfate, filtered and evaporated in vacuo to give 0.3 g (90%) of crude 2-chloro-6-{methyl[(2-methylcyclopropyl)methyl]amino}isonicotinic acid as a brown oil: LCMS (M+H)=255.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07968571B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-99912e004a9944b5a3eb907466340a34 |
| Source note | uspto-grants-2011_06 |