Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | (Diethylamino)sulfur trifluoride | HCID 123472 | — |
| Reactant | HCID 19931990 | HCID 19931990 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19932136 | HCID 19932136 | 95% |
Reaction Steps
20 μl of diethylaminosulfur trifluoride were added at 0° C. to a solution of 54 mg of 1-(diethylcarbamoyl)-3-(2-methyl-3-chlorophenylsulfonyl)-4-hydroxymethylpyrazole (prepared as described in Example 10) in 1.8 ml of methylene chloride, and the resulting mixture was stirred for 1 hour. At the end of this time, the reaction mixture was poured into water and extracted with methylene chloride. 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 concentrate was purified by column chromatography through silica gel, eluted with an 8:1 by volume mixture of hexane and ethyl acetate, to afford 51 mg (yield 95%) of the title compound as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05424279 |
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| Source dataset | uspto-grants-1995_06 |
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| ORD ID | ord-3e37884e66614bbc968e7efc33694788 |
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| Source note | uspto-grants-1995_06 |
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