HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 6-Chloro-2-fluoro-3-(propane-1-sulfonamido)benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Phenylmethyl 3-[bis(propylsulfonyl)amino]-6-chloro-2-fluorobenzoate | HCID 58095375 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Potassium Hydroxide | HCID 14797 | — |
| Product | 6-Chloro-2-fluoro-3-(propane-1-sulfonamido)benzoic acid | HCID 58087500 | 68% |
Reaction Steps
Benzyl 6-chloro-2-fluoro-3-(N-(propylsulfonyl)propylsulfonamido)benzoate (5.4 g, 10.98 mmol) was dissolved in THF (100 mL) and 1M aqueous KOH (100 mL). This mixture was refluxed for 16 hours and then allowed to cool to room temperature. The mixture was then acidified to a pH of 2 with 2M aqueous HCl and extracted with EtOAc (2 X). The extracts were washed with water, dried over sodium sulfate and concentrated to a solid that was triturated with hexanes/ether to give 6-chloro-2-fluoro-3-(propylsulfonamido)benzoic acid (2.2 g, 68%) as a solid. NMR (DMSO-d6, 400 MHz) δ 9.93 (s, 1H), 7.49 (t, 1H, J=8), 7.38 (dd, 1H, J=8, 2), 3.11-3.16 (m, 2H), 1.68-1.78 (m, 2H), 0.97 (t, 3H, J=8).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394795B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-f147378c989f45359b038974dd319569 |
| Source note | uspto-grants-2013_03 |