HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 18179598, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Bromo-1,1-difluoroethane | HCID 136186 | — |
| Reactant | HCID 9914695 | HCID 9914695 | — |
| Product | HCID 18179598 | HCID 18179598 | 33% |
Reaction Steps
To a solution of 261 mg (0.5 mmol) 9-(3,5-bis-trifluoromethyl-benzoyl)-5-(3,4-difluoro-phenyl)-1-oxa-3,9-diaza-spiro[5.5]undecan-2-one in dimethylformamide 24 mg (0.5 mmol) of a 55% sodium hydride suspension in mineral oil was added at room temperature under argon. After 15 min, 80 mg (0.55 mmol) of 2-bromo-1,1-difluoroethane was added. The reaction mixture was stirred at room temperature under argon overnight. After evaporation of the solvent in vacuum water (1 ml) was added and the mixture was extracted with ethyl acetate. The organic layer was dried over (Na2SO4) and concentrated. The residue was purified by column chromatography (SiO2, Hexane/ethylacetate=1:1) to yield 96 mg (33%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06599900B2 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-9520414768c94c518a35e76b29fe4332 |
| Source note | uspto-grants-2003_07 |