HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-Fluoro-6-[(6-trifluoromethyl-pyridin-3-ylmethyl)-amino]-nicotinic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 5-(Aminomethyl)-2-(trifluoromethyl)pyridine | HCID 2737718 | — |
| Reactant | 2,6-Difluoro-nicotinic acid methyl ester | HCID 10844940 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-Fluoro-6-[(6-trifluoromethyl-pyridin-3-ylmethyl)-amino]-nicotinic acid methyl ester | HCID 57619368 | — |
Reaction Conditions
| Temperature | -40 °C |
|---|
Reaction Steps
To 2,6-difluoro-nicotinic acid methyl ester (60, 1.82 g, 0.0105 mol, prepared as described in Example 22, Scheme 24, Step 2) in N,N-dimethylformamide (20.0 mL), under an atmosphere of nitrogen at −40° C., C-(6-trifluoromethyl-pyridin-3-yl)-methylamine (561, 1.00 g, 5.68 mmol) was added. The reaction was stirred at −40° C., then allowed to warm to room temperature for 2 hours. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 35% to 100% ethyl acetate in hexane to give a white solid (562, 1.40 g, 74.9). MS (ESI) [M+H+]+=330.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169250B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-83f1233e6bd74effa51dc4fcfe791c14 |
| Source note | uspto-grants-2015_10 |