Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Azepane | HCID 8119 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 59553060 | HCID 59553060 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59553057 | HCID 59553057 | 33.3% |
Reaction Steps
CDI (63.2 mg, 0.39 mmol) is added to a solution of 2-(4,5,6,7-tetrahydro-1-phenyl-1H-indazol-4-yl)acetic acid (100 mg, 0.39 mmol) in CH2Cl2 (20 mL) cooled in an ice bath, and is heated to 45° C. for 2.5 hours. Then it is cooled to 0° C. and azacycloheptane (38.7 mg, 0.39 mmol) is added and is heated at 45° C. for 1 hour. The solvent is evaporated under reduced pressure, diluted in AcOEt and washed with diluted HCl. The organic phase is dried and evaporated under reduced pressure. The resulting crude product is purified by means of silica gel chromatography, giving 1-(2-(4,5,6,7-tetrahydro-1-phenyl-1H-indazol-4-yl)acetyl)azepane (45 mg, 0.13 mmol, 33%, oil).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07829559B2 |
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| Source dataset | uspto-grants-2010_11 |
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| ORD ID | ord-54432b75e4234c448438c7eea5a72dfc |
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| Source note | uspto-grants-2010_11 |
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