HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → N-(4-iodo-3-methylphenyl)methanesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 4-Iodo-3-methylaniline | HCID 2734275 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-(4-iodo-3-methylphenyl)methanesulfonamide | HCID 58798979 | 94.3% |
Reaction Steps
A solution of 4-iodo-3-methylaniline (4.37 g, 18.75 mmol) in CH2Cl2 (25 ml) was treated with pyridine (6.07 ml, 75 mmol) followed by drop wise addition of methanesulfonyl chloride (1.607 ml, 20.63 mmol) to give a reddish/orange mixture. The mixture was stirred for 2 h, concentrated and diluted with EtOAc. The EtOAc layer was washed with 1M HCl, water, saturated NaCl, dried (Na2SO4) and filtered. The EtOAc filtrate was treated with activated charcoal for 30 min at 50° C. and filtered through a 10 g silica plug and concentrated to give the title compound as a light yellow solid (5.5 g, 94%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09095590B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-4d881551281c4aee8f6a43ac4e62f6d4 |
| Source note | uspto-grants-2015_08 |