HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 58348963, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 8-Azaspiro(4.5)decane | HCID 437152 | — |
| Reactant | Tert-butyldicarbonate | HCID 22064466 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58348963 | HCID 58348963 | 56.3% |
Reaction Steps
To a solution of 8-azaspiro[4.5]decane (which has been described in WO 9800404 A1 6.2 g, 44.5 mmol) in dichloromethane (130 ml), which was cooled to 0° C., triethylamine (7.5 ml, 53.4 mmol) was added then a solution of tert-butyl dicarbonate (10.68 g, 48.9 mmol) in dichloromethane (50 ml) was added in 20 minutes. The clear solution was maintained under stirring at room temperature for 18 hours, then dichloromethane (50 ml) was added and the organic solution was washed with water (2×20 ml), HCl 0.1N (20 ml) then water (2×20 ml). The organic solvent was anhydrified (Na2SO4) and evaporated to give a crude that was purified on silica gel column (Hexane/AcOEt 95/5) to give 6 g of the title compound (light yellow solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859608B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-f9cb358b01454eddb168284c6e3cec27 |
| Source note | uspto-grants-2014_10 |