HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 9839503, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Amino-5-methylbenzoic acid | HCID 76255 | — |
| Reactant | 2,6-Dichlorobenzoyl chloride | HCID 78392 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 9839503 | HCID 9839503 | — |
Reaction Steps
2-Amino-5-methylbenzoic acid (0.5 g) and triethyl amine (10 ml) were mixed in dry toluene (20 ml). 2,6-Dichlorobenzoyl chloride (1.52 g) was added dropwise under cooling and stirring. The mixture was subsequently heated to RT for 24 h, then heated to 80° C. for 1 h. 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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06180625B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-b1e7d460a2ff4914ad51979372bfdce7 |
| Source note | uspto-grants-2001_01 |