HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 22170455, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (Chloromethyl)sulfonyl chloride | HCID 77054 | — |
| Reactant | HCID 10382943 | HCID 10382943 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22170455 | HCID 22170455 | — |
Reaction Steps
The product from Example 3 (500 mg, 1.45 mmol), chloromethanesulfonyl chloride (0.65 g, 4.36 mmol), and triethylamine (1 mL, 7.19 mmol) were stirred in CH2Cl2 (15 mL) overnight at room temperature. The reaction mixture was then diluted with CH2Cl2, washed with H2O and brine, dried over Na2SO4, filtered, and the filtrate concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (99:1 CH2Cl2:CH3OH, eluant) to provide the title compound as a solid. 1H NMR (300 MHz, DMSO-d6) δ 10.31 (s, 1H), 8.87 (dd, J=4.7 Hz, 1.3 Hz, 1H), 8.32 (dd, J=8.2 Hz, 1.7 Hz, 1H), 8.14 (d, J=8.5 Hz, 2H), 7.68-7.77 (m, 3H), 7.38 (d, J=8.8 Hz, 2H), 5.46 (s, 1H), 5.42 (s, 1H), 4.97 (s, 1H), 4.92 (s, 1H), 1.29 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07595332B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-4da0e3ca9e7f4c58adf261a66902f044 |
| Source note | uspto-grants-2009_09 |