HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2,2-Trifluoroethanesulfonyl chloride → HCID 60142919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2,2-Trifluoroethanesulfonyl chloride | HCID 74242 | — |
| Reactant | HCID 70497798 | HCID 70497798 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 60142919 | HCID 60142919 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
A solution of EXAMPLE 65A (18 mg, 0.045 mmol) in dichloromethane (0.4 mL) and pyridine (0.1 mL) was added to a cooled to 0° C. 2,2,2-trifluoroethanesulfonyl chloride (9 mg, 0.05 mmol). The reaction mixture was stirred slowly warming to ambient temperature over 18 hours and concentrated under reduced pressure. The crude material was purified by RP-HPLC (10 mM ammonium acetate/acetonitrile) to afford the title compound. 1H NMR (DMSO-d6) δ ppm 10.27 (s, 1H), 8.21 (d, J=3.0, 1H), 8.14 (d, J=1.9, 1H), 7.68-7.63 (m, 1H), 7.52-7.40 (m, 2H), 7.40-7.33 (m, 2H), 7.30-7.23 (m, 1H), 7.20-7.14 (m, 2H), 7.00-6.94 (m, 2H), 4.54 (q, J=9.8, 2H), 3.13 (m, 4H), 2.45 (m, 4H), 2.24 (s, 3H); MS (ESI) m/z 549 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859546B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-0b8ebd5596474ac2bac0fdf8c7b027ff |
| Source note | uspto-grants-2014_10 |