HuagongsheHuagongshe Chemistry Print Report · For research reference only
Malonic Acid → 1081765-44-7
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Malonic Acid | HCID 867 | — |
| Reactant | 4-Fluoro-3-methoxybenzaldehyde | HCID 2737358 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Piperidine | HCID 8082 | — |
| Product | 1081765-44-7 | HCID 21889850 | 97% |
Reaction Steps
To a solution of 4-fluoro-3-methoxybenzaldehyde (30 g, 195 mmol) in pyridine (134 ml) and piperidine (4.12 ml) was added malonic acid (30.4 g, 292 mmol) at room temperature. The reaction mass was refluxed for 18 h. The solvent was evaporated under reduced pressure and the residue was acidified with 1.5N HCl solution. The precipitated solid was filtered washed with pet ether to get crude compound (37 g, 97%) as white solid. The crude compound was taken to the next step without further purification. 1H NMR (400 MHz, CDCl3): δ ppm 12.37 (s, 1H), 7.59-7.55 (d, J=16 Hz, 1H), 7.53 (s, 1H), 7.26-7.22 (m, 2H), 6.59-6.55 (d, J=16 Hz, 1H), 3.89 (s, 3H); MS: MS m/z 195.0 (M+−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957203B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-df16a25f6c544ae1851707eb1b311400 |
| Source note | uspto-grants-2015_02 |