HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → Methyl 5-chloro-2-(methylamino)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 2-amino-5-chlorobenzoate | HCID 78878 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Methyl 5-chloro-2-(methylamino)benzoate | HCID 12369447 | 13% |
Reaction Steps
A mixture of methyl 2-amino-5-chlorobenzoate (1.0 g, 5.4 mmol), iodomethane (0.75 ml, 12.0 mmol), potassium carbonate (1.7 g, 12.4 mmol), and acetonitrile (20 ml) was stirred for 48 hours. The mixture was filtered through a pad of celite under suction and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography on silica eluting with ethyl acetate-hexane (1:19) to provide 5-chloro-2-methylaminobenzoic acid methyl ester (137 mg, 13% yield) followed by 5-chloro-2-dimethylaminobenzoic acid methyl ester (809 mg, 70% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07291616B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-3dd769ad0d7749b79e96ee72068a5ad6 |
| Source note | uspto-grants-2007_11 |