HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → 4-Chloro-2-(difluoromethyl)-1-(2-{[4-(methylsulfonyl)phenyl]oxy}ethyl)-1H-indole-5-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 4-chloro-2-(difluoromethyl)-1H-indole-5-carbonitrile | HCID 24985632 | — |
| Reactant | 1-(2-Bromoethoxy)-4-methanesulfonylbenzene | HCID 43806954 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 4-Chloro-2-(difluoromethyl)-1-(2-{[4-(methylsulfonyl)phenyl]oxy}ethyl)-1H-indole-5-carbonitrile | HCID 24986126 | 61.6% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
To a solution of 4-chloro-2-(difluoromethyl)-1H-indole-5-carbonitrile (0.019 g, 0.084 mmol) in MeCN (2 mL), under N2, was added Cs2CO3 (0.055 g, 0.17 mmol) and 4-[(2-bromoethyl)oxy]phenyl methyl sulfone (0.047 g, 0.17 mmol). The mixture was heated in a sealed tube at 100° C. for 1 h. Upon cooling, the mixture was partitioned between EtOAc and water. The organic phase was washed with sat'd brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by flash chromatography (0-70% EtOAc-hexanes gradient) and the product was crystallized from CH2Cl2-hexanes to give the title compound as a white solid (0.022 g, 61% yield): MS (ES) m/z 425 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673948B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-6fc237df39514f6d8623a3d7d00c1f57 |
| Source note | uspto-grants-2014_03 |