HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 21948300, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Amino-4-chloropyridine | HCID 581866 | — |
| Reactant | HCID 21948280 | HCID 21948280 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 21948300 | HCID 21948300 | 20.8% |
Reaction Steps
2-Amino-4-chloropyridine (132 mg), triethylamine (700 mg) and ethanol (15 ml) were added to 1-{[4-ethoxycarbonylamino-4-piperidinyl]methyl}-4-(4-vinylbenzensulfonyl)-2-piperazinone hydrochloride (250 mg), to react at 155° C. for 20 hours in a sealed tube. The reaction solution was concentrated, a 10% aqueous sodium carbonate solution was added to the residue, the material was extracted with dichloromethane, dried, and concentrated. The resulting residue was dried, concentrated, purified by column chromatography (dichloromethane:10% aqueous ammonia-containing methanol=20:1), and crystallized from dichloromethane-hexane to obtain the title compound (58 mg) as pale yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07109200B2 |
| Source dataset | uspto-grants-2006_09 |
| ORD ID | ord-2f7ecb92e34348f98281fd809f5a3ab3 |
| Source note | uspto-grants-2006_09 |