HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 117697851, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | tert-Butoxy bis(dimethylamino)methane | HCID 79885 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 9-Boc-7-oxa-9-azabicyclo[3.3.1]nonan-3-one | HCID 18507052 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 117697851 | HCID 117697851 | 100% |
Reaction Steps
A solution of tert-butyl 7-oxo-3-oxa-9-azabicyclo[3.3.1]nonane-9-carboxylate (482 mg, 2 mmol) and tert-butoxy-N,N,N′,N′-tetra-methyl-methanediamine (522 mg) in dioxane (10 mL) was stirred at 60° C. for 16 h. The solvent was removed in vacuo, and the residue was dissolved in EtOH (10 mL). To it NH2OH.HCl (462 mg, 3 mmol) was added. After stirring at room temperature for 2 h, 12 N HCl (1 mL) was added and refluxed for 2 h. The reaction mixture was concentrated to give 5,10-Dioxa-4,12-diaza-tricyclo[6.3.1.0*2,6*]dodeca-2(6),3-diene 105a as an oil (yield 100%), which was used without further purification. MS: calc'd (MH+) 167, measured (MH+) 167.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09266904B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-018f6cb6c47b40129be8594c05344b1e |
| Source note | uspto-grants-2016_02 |