HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 24853167, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 15451838 | HCID 15451838 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24853167 | HCID 24853167 | — |
Reaction Steps
The imine (Example 26A, 30 mg, 0.09 mmol) was dissolved in dichloromethane (1.5 mL). Diisopropylethylamine (31 μl, 0.18 mmol, 2 equiv.) was added followed by the methanesulfonyl chloride (0.1 mmol, 1.1 equiv.). The reaction was stirred at room temperature for 4 hours. The reaction mixture was passed through a Si-amine cartridge (1 g, 1.6 mmol/g) to remove the excess sulfonyl chloride and washed with additional dichloromethane. The resulting solution was dried, concentrated, and purified by reverse phase HPLC. 1H NMR (500 MHz, DMSO-d6) δ ppm 2.24 (3H), 2.90-2.96 (3H), 7.31 (1H), 7.56 (1H), 7.68 (1H), 7.8 (1H); MS (ESI) m/z 398.9 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07683084B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-6084fc16c881429bbc0a77e4491eb439 |
| Source note | uspto-grants-2010_03 |