Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 87840440 | HCID 87840440 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 86604719 | HCID 86604719 | — |
Reaction Steps
770 μL (5.52 mmol) of triethylamine are added to a solution of hydroxylamine hydrochloride (384 mg, 5.52 mmol) in 1.8 ml of DMSO, and the suspension is stirred for 20 minutes at ambient temperature. The precipitate is filtered off and the filtrate is concentrated in vacuo. To the resulting filtrate there are added 225 mg (0.921 mmol) of the compound of Step A above and the solution is stirred at 75° C. for 4 hours. The reaction mixture is cooled to ambient temperature and the reaction mixture is precipitated from water. A white, non-filterable, gummy paste is obtained which is separated from the aqueous phase by simple decanting. The gum is triturated in ethanol until crystallisation occurs. The solid is filtered off to yield the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07268130B2 |
|---|
| Source dataset | uspto-grants-2007_09 |
|---|
| ORD ID | ord-9209a028860048ea8bb005a9ce38c81e |
|---|
| Source note | uspto-grants-2007_09 |
|---|