HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → Ethyl 2-amino-3-bromo-5-methylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 2-Amino-3-bromo-5-methylbenzoic acid | HCID 2774400 | — |
| Product | Ethyl 2-amino-3-bromo-5-methylbenzoate | HCID 54594338 | 64% |
Reaction Steps
Ethanol (10 mL) was added to 2-amino-3-bromo-5-methylbenzoic acid (1.00 g, 4.4 mmol). While the mixture was stirred, thionyl chloride (1.03 g, 8.7 mmol) was added at room temperature, followed by stirring at 80° C. overnight. The reaction solution was concentrated, and then diluted with water under ice-cooling, followed by extraction with ethyl acetate. The organic layer was washed with aqueous sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane=0/10, 4/6) to obtain 715 mg of the title compound as a pale yellow solid (64%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08927588B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-536cf4a9793244299424c2221607ffff |
| Source note | uspto-grants-2015_01 |