HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → HCID 145785766, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 86598909 | HCID 86598909 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 145785766 | HCID 145785766 | 77.3% |
Reaction Steps
To a solution of tert-butyl (1R,3S,4S,6R)-3-{[(2S)-2-cyano-1-pyrrolidinyl]carbonyl}-6-(2-oxoethoxy)-2-azabicyclo[2.2.1]heptane-2-carboxylate obtained in Example 25-1 (163 mg) in ethanol (6 mL) and water (1 mL), were added hydroxylamine hydrochloride (36 mg) and sodium acetate (46 mg). The mixture was stirred at reflux for 20 minutes. To the resulting mixture, brine was added. The mixture extracted with ethyl acetate. The combined organic phase was washed with brine, dried over sodium sulfate, and evaporated in vacuo. The residue was chromatographed on silica gel eluting with ethyl acetate to give the target compound (131 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07186731B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-296392ba0206409894205b3b215ceae1 |
| Source note | uspto-grants-2007_03 |