Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Sodium methanesulfinate | HCID 2733271 | — |
| Reactant | HCID 117840596 | HCID 117840596 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131734075 | HCID 131734075 | 23.9% |
Reaction Steps
To a solution of the crude 2-(4-((tert-butoxycarbonyl)amino)-1H-pyrazol-1-yl)-2-methylpropyl methanesulfonate (1.1 g) obtained in Step B of Example 114 in N,N-dimethylformamide (10 mL) were added sodium iodide (740 mg) and sodium methanesulfinate (1.0 g), and the mixture was stirred overnight at 140° C. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (250 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09187453B2 |
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| Source dataset | uspto-grants-2015_11 |
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| ORD ID | ord-f42fb3f593c14956b5cd043d8cb809d0 |
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| Source note | uspto-grants-2015_11 |
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