HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → 2-Ethanoyloxy-5-tert-butoxycarbonylaminobenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-(N-tert-Butoxycarbonylamino)salicylic Acid | HCID 10377562 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-Ethanoyloxy-5-tert-butoxycarbonylaminobenzoic acid | HCID 22341901 | 52.2% |
Reaction Steps
To a solution of 5-tert-butoxycarbonylamino-2-hydroxybenzoic acid (1.02 g, 4.02 mmole) in DMF (20.0 ml) was added with acetyl chloride (39 mg, 4.83 mmole) and potassium carbonate (555 mg, 4.02 mmole). The reaction mixture was stirred for 4 hr at room temperature. After the reaction mixture was concentrated, the residue was dissolved in ethyl acetate. The organic layer was washed with water and brine and dried over anhydrous Na2SO4. After evaporation of the solvent, the residue was recrystallized from ethyl acetate/hexane to give 0.62 g (52% yield) of 2-ethanoyloxy-5-tert-butoxycarbonylaminobenzoic acid as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06927303B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-ae905d21ae4948efa3b1e5e5206e6565 |
| Source note | uspto-grants-2005_08 |