Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 86696276 | HCID 86696276 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 71536919 | HCID 71536919 | 64.7% |
Reaction Steps
To a solution of (77.3) (10 mg, 0.025 mmol) and hydroxylamine hydrochloride (6.86 mg, 0.099 mmol) in EtOH (5 ml) was added 0.01 ml of HCl (2 N) and the mixture was stirred in a sealed tube at 80° C. overnight. The mixture was evaporated to dryness and dissolved in H2O again, which was neutralized immediately by NaHCO3 until pH reached about 9. The resulted precipitate was filtered quickly. The precipitate was dissolved in DCM/MeOH (10/1) and washed again by water. The organic phase was dried over Na2SO4, filtered and evaporated to give the title compound (6.8 mg, yield 60.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09062045B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-0a42f96d479041dda8a2cd403f4bc62e |
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| Source note | uspto-grants-2015_06 |
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