HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86757743, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 70161361 | HCID 70161361 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86757743 | HCID 86757743 | 29.6% |
Reaction Steps
To a solution of 200 mg of (Z)-1-{[4,4-difluoro-1-(4-methyl-2-phenylthiazole-5-carbonyl)-2,3,4,5-tetrahydro-1H-1-benzoazepin-5-ylidene]acetyl}piperidin-4-one in a mixture of 6 ml of dichloromethane and 3 ml of methanol were added 29 mg of hydroxylamine monohydrochloride and 59 μl of triethylamine, followed by stirring at room temperature for 22 hours. After evaporating the solvent, the residue was purified by silica gel column chromatography (eluting with chloroform-methanol), followed by crystallizing from diethyl ether to give 61 mg of (Z)-4,4-difluoro-5-{2-[4-(hydroxyimino)piperidino]-2-oxo-ethylidene}-1-(4-methyl-2-phenylthiazole-5-carbonyl)-2,3,4,5-tetrahydro-1H-1-benzoazepine as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06340678B1 |
| Source dataset | uspto-grants-2002_01 |
| ORD ID | ord-596513dc5e414ec7a47505527fd2f0fe |
| Source note | uspto-grants-2002_01 |