HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → Methyl 2-{[(3-{[2-(trimethylsilyl)ethoxy]carbonyl}phenyl)sulfonyl]amino}benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Methyl Anthranilate | HCID 8635 | — |
| Reactant | 2-(Trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate | HCID 86676334 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | Methyl 2-{[(3-{[2-(trimethylsilyl)ethoxy]carbonyl}phenyl)sulfonyl]amino}benzoate | HCID 71238679 | 92.2% |
Reaction Steps
To a mixture of 2.09 g of 2-(trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate and 20 mL of methylene chloride were added 982 mg of methyl 2-aminobenzoate and 2.10 mL of pyridine under ice-cooling, followed by stirring at room temperature for 15 hours. To the reaction mixture was added a 10% aqueous citric acid solution, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 2.61 g of methyl 2-{[(3-{[2-(trimethylsilyl)ethoxy]carbonyl}phenyl)sulfonyl]amino}benzoate as a colorless oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09284295B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-85f77c7d02fa4c4e97559078b7e23ae5 |
| Source note | uspto-grants-2016_03 |