HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → N-(6-iodopyridin-3-yl)methanesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 6-Iodopyridin-3-amine | HCID 2320576 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-(6-iodopyridin-3-yl)methanesulfonamide | HCID 86652124 | 100% |
Reaction Steps
To a solution of 6-iodopyridin-3-amine (1.077 gm, 4.90 mmole) in dichloromethane (40 ml) and pyridine (1.98 ml, 24.49 mmole) at ice bath temperature was added methanesulfonyl chloride (0.401 ml, 2.444 mmole). The mixture was allowed to warm to room temperature and stir four days. The reaction mixture was treated with 5% acetic acid and allowed to stir 20 min at room temperature. The organic phase was washed with water (2×50 ml), dried (MgSO4) and concentrated in vacuo. The residue was slowly added in portions to rapidly stirred water (100 ml) and the resulting solid collected by filtration, washed with water and dried in vacuo to give the title compound (0.7287 g, 49.9%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09095590B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-5fd46ea177134ea3aff88c1df7741a4e |
| Source note | uspto-grants-2015_08 |