HuagongsheHuagongshe Chemistry Print Report · For research reference only
(Diethylamino)sulfur trifluoride → 2-(3-Chlorophenyl)-2-fluoro-1-[4-(dimethylamino)phenyl]ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (Diethylamino)sulfur trifluoride | HCID 123472 | — |
| Reactant | 2-(3-Chlorophenyl)-2-hydroxy-1-[4-(dimethylamino)phenyl]ethanone | HCID 15728476 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(3-Chlorophenyl)-2-fluoro-1-[4-(dimethylamino)phenyl]ethanone | HCID 15728478 | — |
Reaction Steps
A solution 6.7 g diethylaminosulfur trifluoride in 20 ml of dry dichloromethane was stirred at -78° C. under nitrogen as a solution of 12 g of 2-(3-chlorophenyl)-2-hydroxy-1-[4-(dimethylamino)phenyl]ethanone in 200 ml of dry dichloromethane was added dropwise. The mixture was warmed to room temperature and stirred for 72 hours. The mixture was poured into 200 ml of ice water and the layers separated. The organic layer was dried (Na2SO4), filtered, and evaporated. The residue was purified by flash chromatography (8:1 hexane-ethyl acetate) and then recrystallized from ether-hexane to give 1.1 g of 2-(3-chlorophenyl)-2-fluoro-1-[4-(dimethylamino)phenyl]ethanone, mp 90°-92° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05177111 |
| Source dataset | uspto-grants-1993_01 |
| ORD ID | ord-5686aff2d2964967988f2361ff02037c |
| Source note | uspto-grants-1993_01 |