HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 86710508, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2,2,2-Trifluoroethyl trifluoromethanesulfonate | HCID 80366 | — |
| Reactant | HCID 66582827 | HCID 66582827 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86710508 | HCID 86710508 | 63.8% |
Reaction Steps
At 0° C., NaH (1.6 g) was added into a solution of (5-bromo-2-chlorophenyl)(4-hydroxyphenyl)methanone (6.2 g) in dry DMF (40 mL). The mixture was stirred at room temperature for 1 h. Then CF3CH2OTf (9.3 g) was slowly added into the mixture at 0° C. The mixture was stirred at room temperature for 0.5 h. Saturated NH4Cl aqueous solution was added slowly into the mixture, and the mixture was extracted with EtOAc. The organic phases were combined, dried over Na2SO4 and concentrated to obtain the crude product, then the crude product was purified by silica-gel column chromatography (PE/EA=20/1) to obtain 5.0 g of (5-bromo-2-chlorophenyl)(4-(2,2,2-trifluoroethoxy)phenyl)methanone.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957033B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-378eba0574704947aece7541954c7f13 |
| Source note | uspto-grants-2015_02 |