Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 58042365 | HCID 58042365 | — |
| Reactant | 5-chloro-2,4-difluoro-N-(methylsulfonyl)benzamide | HCID 58042417 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58042370 | HCID 58042370 | 8.7% |
Reaction Steps
Sodium hydride (60% in mineral oil, 0.012 g, 0.306 mmol) was added to a solution of 1-isopropyl-1H-indazol-5-ol (Preparation 39, 0.045 g, 0.225 mmol) in THF (3.0 mL) while cooling the reaction in an ice bath and stirred for 40 minutes. 5-Chloro-2,4-difluoro-N(methylsulfonyl)benzamide (Preparation 28, 0.076 g, 0.28 mmol) was then added and the reaction was heated at 60° C. for 16 hours. The reaction mixture was concentrated in vacuo and the residue treated with EtOAc (25.0 mL) and washed with water (30.0 mL), followed by brine (30.0 mL). The organic layer was dried over sodium sulfate, filtered, concentrated in vacuo and the residue purified by silica gel chromatography eluting with 2% Methanol in DCM to yield the title compound as a white solid (8.3 mg):
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08592629B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-ee843dd39a8542e5b37a0db4e450cea8 |
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| Source note | uspto-grants-2013_11 |
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