HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 58313162, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | HCID 58313067 | HCID 58313067 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58313162 | HCID 58313162 | 29% |
Reaction Steps
Ethyl 8-oxa-2-azaspiro[4.5]decane-3-carboxylate (3.54 g, 16.6 mmol) was dissolved in dry dichloromethane (80 mL), triethylamine (5.8 mL, 41.5 mmol) was added followed by benzylchloroformate (3.5 mL, 24.9 mmol) and the reaction is stirred at room temperature for 2 h under nitrogen. The reaction was diluted with dichloromethane, washed with 0.2 N HCl, dried over MgSO4 and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with 20-100% hexanes/EtOAc to afford a yellow oil. The racemate was then separated by chiral HPLC on a 10 μm OD column eluting with 25% isopropanol in hexanes to afford the title compound as a clear oil (1.66 g, 29% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08492554B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-90caa45c04854bb1926082923d97077c |
| Source note | uspto-grants-2013_07 |