Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 19886494 | HCID 19886494 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57010991 | HCID 57010991 | 22.2% |
Reaction Steps
960 mg (0.24 mmole) of sodium hydride (as a 60% w/w dispersion in mineral oil) were added, whilst ice-cooling, to a solution of 77.9 mg (0.2 mmole) of 2-(2,4-difluorophenyl)-4-methanesulfonyloxy-3-methyl-1-(1H-1,2,4-triazol-1-yl)-2-hexanol in 4.9 ml of dimethylformamide. The resulting mixture was then stirred at room temperature for 3 hours. At the end of this time, the reaction mixture was poured into 20 ml of ice-water and extracted with 40 ml of ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated by evaporation under reduced pressure. The residue was purified by preparative thin layer chromatography, using a 2:1 by volume mixture of hexane and ethyl acetate as the developing solvent, to afford 13.0 mg (yield 22.2%) of the title compound as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05134152 |
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| Source dataset | uspto-grants-1992_07 |
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| ORD ID | ord-eca1c225af8c40548273e6ec56d3ca30 |
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| Source note | uspto-grants-1992_07 |
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