Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | PyBOP | HCID 2724699 | — |
| Reactant | Methylamine hydrochloride | HCID 6364545 | — |
| Reactant | HCID 58138764 | HCID 58138764 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ammonium Chloride | HCID 25517 | — |
| Product | HCID 58138839 | HCID 58138839 | — |
Reaction Steps
To a solution of 3-({[1-(4-fluoro-phenyl)-1H-indazole-4-carbonyl]-amino}-methyl)-benzoic acid (70 mg, 0.2 mmol) in DMF (5 mL) was added Et3N (0.07 mL, 0.6 mmol) and PyBOP (100 mg, 0.2 mmol). After 15 minutes of stirring at room temperature, methylamine hydrochloride (15 mg, 0.22 mmol) was added. After 16 hours, the mixture was diluted with saturated aqueous ammonium chloride (20 mL) and extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with saturated aqueous sodium bicarbonate (20 mL), brine (20 mL) and dried over sodium sulfate. The crude product was purified by silica gel chromatography eluting with a gradient of 0-100% ethyl acetate in hexanes. The material from the column was then crystallized from EtOAc/ether/hexanes to afford the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08008327B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-2a47ba1b22c84e46a6870d4ed69bb389 |
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| Source note | uspto-grants-2011_08 |
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