Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 66767109 | HCID 66767109 | — |
| Reactant | HCID 66767154 | HCID 66767154 | — |
| Solvent | Ethanol ethylacetate | HCID 21584252 | — |
| Product | HCID 66767128 | HCID 66767128 | 265.6% |
Reaction Steps
To a solution of 5-(2-fluoro-4-nitrophenoxy)-6-(1H-pyrazol-4-yl)-1-(tetrahydropyran-2-yl)-1H-indazole (900 mg, 2.13 mmol) and 4-[5-(2-fluoro-4-nitro-phenoxy)-1-(tetrahydropyran-2-yl)-1H-indazol-6-yl]-pyrazole-1-carboxylic acid tert-butyl ester (3.1 g, 5.92 mmol) in EtOAc/EtOH (75 mL/75 mL) is added stannous chloride dihydrate (10 g, 52.74 mmol). The reaction mixture is stirred at reflux overnight. After it is cooled and basified with saturated aqueous NaHCO3 to pH 8-9, the mixture is extracted with EtOAc (100 mL). The organic phase is separated, dried over MgSO4, and concentrated. The residue is purified by silica gel column chromatography eluting first with PE:EtOAc (1:1) and then with EtOAc to give the product (1.75 g, 71.0% yield). MS (m/z): 310.0 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08030302B2 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-5536e1d65ebc4b8cb34fe2aa7299cb34 |
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| Source note | uspto-grants-2011_10 |
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