HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 8-tert-Butyloxycarbonyl-2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,8-Diazaspiro(4,5)decane-1,3-dione, 2-methoxy-, monohydrochloride | HCID 3088285 | — |
| Reactant | Tert-butyldicarbonate | HCID 22064466 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 8-tert-Butyloxycarbonyl-2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione | HCID 14371816 | — |
Reaction Steps
To a solution of 2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione hydrochloride (1.5 g) in dimethylformamide (100 ml) was added triethylamine (1 ml), followed by tert-butyl dicarbonate (2.05 ml), and this was followed by stirring at room temperature for 1 hour. The solvent was evaporated off under reduced pressure. To the residual oil dichloromethane (50 ml) was added, after which it was washed with a 10% aqueous solution of citric acid, then with water. After drying the organic layer with anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure. The resulting residual solid was recrystallized with ethyl ether to obtain 1.4 g of a colorless crystal having a melting point of 117° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04804665 |
| Source dataset | uspto-grants-1989_02 |
| ORD ID | ord-365fe5725d1a447e86ca99febdd6a34b |
| Source note | uspto-grants-1989_02 |