HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Fluorobenzylamine → HCID 54724205, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Fluorobenzylamine | HCID 66853 | — |
| Reactant | 4-Hydroxy-6-methyl-2-pyrone | HCID 54675757 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 54724205 | HCID 54724205 | 18.4% |
Reaction Steps
A mixture of 4-hydroxy-6-methyl-2-pyrone (2.5 g, 0.02 mol) and 3-fluorobenzylamine (2.5 g, 0.02 mol) in n-butanol (15.0 mL) was heated to reflux for 16 h under argon atmosphere. Butanol wad distilled in vacuo, the residue was triturated with EtOAc, cooled and filterd the precipitate. It was washed with cold EtOAc, and dried to give 0.86 g of the title compound as a pale yellow powder: 1H-NMR (CD3OD/400 MHz) δ 7.31 (m, 1H), 7.0-6.85 (m, 2H), 6.83 (d, 1H, J=9.6 Hz), 5.96 (d, 1H, j=2.0 Hz), 5.80 (d, 1H, J=2.0 Hz), 5.30 (s, 2H), and 2,24 (s, 3H); ES MS m/z 234 (MH+). Step 2: Preparation of 3-bromo-1-(3-fluorobenzyl)-4-hydroxy-6-methylpyridin-2(1H)-one
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07067540B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-96214eac87294e609aaef56fc34cd4f0 |
| Source note | uspto-grants-2006_06 |