HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → N-[2-(4-propionylamino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide oxalate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Propionyl chloride | HCID 62324 | — |
| Reactant | N-[2-(4-amino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide dioxalate | HCID 86751129 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-[2-(4-propionylamino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide oxalate | HCID 18969240 | — |
Reaction Steps
The product from Example 23, as the free base (0.310 g, 0.94 mmol) and triethylamine (0.13 mL, 0.94 mmol) were stirred in 10.0 mL tetrahydrofuran and cooled briefly in an ice bath. To the mixture was added dropwise propionyl chloride (0.08 mL, 0.94 mmol) and the resulting mixture was stirred 18 h at room temperature and filtered, and the filtrate was evaporated to an oil. Crystallization as the oxalate salt from ethyl acetate/methanol provided 0.168 g colorless crystals. Mp 169° C. Mass spectrum, m+ =385. Anal (C23H33N5O6) theory C, 58.09; H, 6.99; N, 14.73; found C, 57.79; H, 6.93; N, 14.46.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05654320 |
| Source dataset | uspto-grants-1997_08 |
| ORD ID | ord-4adb00e91ad24e6caf3e450e93a7b73a |
| Source note | uspto-grants-1997_08 |