HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 21069935, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | 5-Fluoro-2-methylbenzenesulphonyl chloride | HCID 136286 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 21069935 | HCID 21069935 | 96% |
Reaction Steps
To a solution of 5-fluoro-2-methyl-benzenesulfonyl chloride (4.18 g, 20 mmol) in acetone (20 mL) was added a 40% aqueous solution of methylamine (4.5 mL, 60 mmol) under nitrogen and the mixture stirred for 5 min. Acetone was removed in vacuo and the aqueous residue extracted with CH2Cl2. The CH2Cl2 extract was dried (Na2SO4), filtered, concentrated and the residue purified by column chromatography (SiO2, 10% ether in CH2Cl2) to provide 3.9 g (19.2 mmol, Yield 96%) of the title compound as a white solid; 1H NMR (500 MHz, CDCl3) δ ppm: 2.59 (3H, s), 2.67 (3H, d, J=5.5 Hz), 4.41 (1H, brs), 7.13–7.20 (1H, m), 7.29 (1H, dd, J=8.2, 5.5 Hz), 7.69 (1H, J=8.6, 2.1 Hz); LC/MS m/z 204 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176196B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-203822cb835e4bbfa21398de4802239f |
| Source note | uspto-grants-2007_02 |