Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 178473418 | HCID 178473418 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 89666817 | HCID 89666817 | 46.8% |
Reaction Steps
Iodomethane (10 ml) and cesium carbonate (4.89 g) were added to an acetone (20 ml) solution containing ethyl 3-hydroxy-5-nitro-1H-indazol-1-carboxylate (2.51 g) obtained in the 2nd step under ice cooling in a nitrogen atmosphere, followed by stirring at 80° C. for 0.5 hours. An insoluble precipitate was removed by filtration and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0 to 4:1). A white solid of ethyl 3-methoxy-5-nitro-1H-indazol-1-carboxylate (1.24 g) was thus obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09051310B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-4fae5d3ae55b41bb9d7f4ab87969c6f5 |
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| Source note | uspto-grants-2015_06 |
|---|