HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → N-Boc-hexahydro-1H-azepin-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Azepan-4-one | HCID 1501891 | — |
| Reactant | Tert-butyldicarbonate | HCID 22064466 | — |
| Solvent | 2-Methylpropan-2-ol--water (1/1) | HCID 71401949 | — |
| Product | N-Boc-hexahydro-1H-azepin-4-one | HCID 1512679 | 84% |
Reaction Steps
To a stirred solution of 4-oxohomopiperidine.HCl (1.2 g, 8.05 mmol), NaOH (0.68 g, 16.9 mmol) in t-BuOH/H2O (1:1, 10 mL) was added t-butyldicarbonate (1.93 mL, 8.9 mmol) drop-wise. The reaction was stirred at RT overnight, extracted with EtOAc (2×10 mL) and the organic layer separated. The organic layer was dried over Na2SO4 and concentrated under vacuo. Pure 1-t-butoxycarbonyl-4-oxohomopiperidine (1.42 g, 84%) was isolated via silica gel flash chromatography eluting with 50% EtOAc/hexane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653096B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-72a38cefc93941b9a6a7785939b5cf2a |
| Source note | uspto-grants-2014_02 |