HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → Methyl 5-[(tert-butoxycarbonylamino)methyl]-2-chloro-benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-(((tert-Butoxycarbonyl)amino)methyl)-2-chlorobenzoic acid | HCID 58483357 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Methyl 5-[(tert-butoxycarbonylamino)methyl]-2-chloro-benzoate | HCID 86692228 | 41.9% |
Reaction Steps
To a solution of 5-{[(tert-butoxycarbonyl)amino]methyl}-2-chlorobenzoic acid (1.0 g, 3.50 mmol) in DMF (5.0 mL) were added methyl iodide (496 mg, 3.50 mmol) and K2CO3 (966 mg, 7.00 mmol). The reaction mass was stirred at rt for 18 h. The reaction mass was diluted with EtOAc and the organic layer was washed with water and brine. The organic layer was separated, dried, filtered and concentrated. The concentrate was purified by column chromatography to afford 440 mg of the title product. 1H NMR (300 MHz, DMSO d6): δ 7.66 (s, 1H), 7.49-7.52 (m, 2H), 7.42 (d, J=6.3 Hz, 1H), 4.13 (d, J=5.7 Hz, 2H), 3.85 (s, 3H), 1.38 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006257B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-ebb8759a32ff44b8be66a10cea2d4e20 |
| Source note | uspto-grants-2015_04 |