HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 15986633, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 57833605 | HCID 57833605 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15986633 | HCID 15986633 | — |
Reaction Steps
A solution of 1-{3-[4-(benzhydrylidene-amino)-xanthen-9-ylidene]-8-aza-bicyclo[3.2.1]oct-8-yl}-2,2,2-trifluoroethanone in methanol (0.1 to 1 M solution) may be treated with sodium acetate (2 to 4 equiv) and hydroxylamine hydrochloride (1 to 3 equiv) and stirred at rt for 1 to 4 days. Sodium hydroxide may be added to make the solution basic, and the solution may be stirred at rt for 1 to 5 hr. Methylene chloride and water may be added, and the organic layer may be separated. After drying over a suitable drying agent such as potassium carbonate, filtration, and evaporation, the residue may be purified via reverse phase column chromatography to yield Compound 2c.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07582650B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-25abc55c8cdf409ab1762c323dfcd4af |
| Source note | uspto-grants-2009_09 |