HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 69978127, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sulfamic Acid | HCID 5987 | — |
| Reactant | Methyl Acrylate | HCID 7294 | — |
| Reactant | 4-Fluoroanthranilic acid | HCID 2724967 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Catalyst | Palladium acetylacetonate | HCID 5486778 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 69978127 | HCID 69978127 | 76.1% |
Reaction Steps
At 0C, a solution of 0.52 g of sodium nitrite in 1 ml of water is added within a period of 30 minutes to a mixture of 1 g of 2-amino-4-fluorobenzoic acid, 15 ml of water and 6.24 ml of concentrated sulfuric acid. The mixture is then stirred for one hour. Following addition of 0.3 g of amidosulfonic acid, 0.7 g of methyl acrylate in 9 ml of isopropanol are added dropwise, and 10 mg of palladium acetylacetonate are added. After 4 hours at 40° C., 30 ml of water are added and the resulting precipitate is filtered off. Drying gives 1.1 g of 4-fluoro-2-(3-methoxy-3-oxo-1-propenyl)-benzoic acid of melting point 151-153° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06455725B1 |
| Source dataset | uspto-grants-2002_09 |
| ORD ID | ord-87856a5e97a944ef949ffef218558d37 |
| Source note | uspto-grants-2002_09 |