HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Fluorobenzylamine → HCID 81751143, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Fluorobenzylamine | HCID 66649 | — |
| Reactant | 3-Fluoropyridine-4-carboxylic acid | HCID 345361 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 81751143 | HCID 81751143 | 10.3% |
Reaction Conditions
| Temperature | 158 °C |
|---|
Reaction Steps
3-Fluoroisonicotinic acid (100 mg, 0.71 mmol) and 2-fluorobenzylamine (308 μL, 2.84 mmol) were combined in ACN (3 mL) and the solution was stirred at 158° C. in a microwave for 1 h. The solution was concentrated in vacuo and purified by silica gel chromatography (10% to 20% MeOH/DCM). The semi-pure fractions were concentrated and then taken up in water to give a white precipitate, which was collected by filtration and dried under vacuum to give 18 mg (10%) of the title compound. 1H NMR (500 MHz, DMSO-d6): δ 8.18 (s, 1H), 7.99 (br s, 1H), 7.84 (d, 1H, J=5.0 Hz), 7.58 (d, 1H, J=5.0 Hz), 7.31-7.41 (m, 2H), 7.15-7.23 (m, 2H), 4.62 (s, 2H). [M+H] calc'd for C13H11FN2O2, 247. found 247.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447045B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-693f9bedb57c4f69bf39d51a4643c9ad |
| Source note | uspto-grants-2016_09 |