Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydroxylamine | HCID 787 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 18438954 | HCID 18438954 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 136251062 | HCID 136251062 | — |
Reaction Steps
A solution of 8 (16 mmol), hydroxylamine hydrochloride (10 eq, 11.2 g) and pyridine (270 mL) was heated to 80° C. for 24 hours. Additional hydroxylamine (3 g) was added and the temperature increased to 90° C. After LC analysis confirmed the consumption of starting material, the reaction was cooled and the pyridine removed by rotary evaporation. The residue was dissolved in DCM and washed with water and 1M HCl. The organic layer was dried over Na2SO4 and concentrated. The reaction mixture was purified by flash chromatography eluding with 20% EtOAc/hexanes, Rf=0.4. The product was isolated as a white foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07186746B2 |
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| Source dataset | uspto-grants-2007_03 |
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| ORD ID | ord-c5e15df36bef44bfb37ac448b8b839e8 |
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| Source note | uspto-grants-2007_03 |
|---|