HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 58020013, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 58020122 | HCID 58020122 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58020013 | HCID 58020013 | 55% |
Reaction Steps
To a 4 mL vial was added P-255 (60 mg, 0.17 mmol), followed by pyridine (2 mL) then methanesulfonyl chloride (13 μL) at 0° C. The resulting solution was allowed to stir at room temperature overnight. The reaction mixture was diluted with water (10 mL) and extracted with ethyl acetate (3×5 mL). The combined organics were concentrated under vacuum, and the residue was purified by silica gel column chromatography with methanol/dichloromethane to yield 36.7 mg (55%) of P-271). 1H NMR (400 MHz, CDCl3) 2.98 (s, 3H), 3.79 (s, 3H), 3.94 (s, 2H), 6.53 (s, 1H), 6.91 (d, J=8.4 Hz, 1H), 6.99-7.17 (m, 5H), 7.22-7.35 (m, 3H), 7.34-7.41 (m, 1H), 7.48 (s, 1H) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08791267B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-c367209e4e1542588e43612588639c88 |
| Source note | uspto-grants-2014_07 |