HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67345591, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2-Hydroxy-3-methylpyridine | HCID 70481 | — |
| Reactant | 2,2,2-Trifluoroethyl trichloromethanesulphonate | HCID 90027 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67345591 | HCID 67345591 | 55.9% |
Reaction Steps
Cesium carbonate (11.4 g, 34.9 mmol) was added to a solution of 3-methylpyridin-2(1H)-one (3.81 g, 34.9 mmol) and 2,2,2-trifluoroethyl trichloromethanesulfonate (9.81 g, 34.9 mmol) in dichloromethane (80 mL). After 2 h, water was added. The mixture was extracted with ether (3×), and the combined organic extracts were dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% dichloromethane 25%→methanol/dichloromethane) gave the title compound (3.73 g). MS192.3 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07994325B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-3c6993b09bf7430d96205b6c20ca703a |
| Source note | uspto-grants-2011_08 |