HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 9861484, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Fluorobenzoyl chloride | HCID 9808 | — |
| Reactant | 2-Amino-3,6-dichlorobenzoic acid | HCID 604542 | — |
| Solvent | Ethylacetate heptane | HCID 21899848 | — |
| Product | HCID 9861484 | HCID 9861484 | — |
Reaction Steps
2-Amino-3,6-dichlorobenzoic acid (0.5 g) and triethyl amine (20 ml) were mixed. 2-Fluorobenzoyl chloride (0.77 g) was added dropwise under cooling and stirring. The mixture was subsequently heated to RT and stirred until disappearance of starting material was seen on TLC (silicagel) using heptane/ethyl acetate (4/1) as eluent. After cooling on ice the precipitate was filtered off and the filtrate evaporated to dryness. The residue was partitioned between methylene chloride and potassium carbonate (2N), the organic layers separated, dried over magnesium sulfate and evaporated to dryness. The raw product was purified by column chromatography on silicagel using heptane/ethyl acetate as eluent. Yield 0.31 g. m.p. 140° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06180625B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-99e52a8203e14f49a27bf165a2bcb35f |
| Source note | uspto-grants-2001_01 |