HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 1-azabicyclo(2.2.2)octane-4-carboxylate → 1-Azabicyclo[2.2.2]oct-4-yl[bis(3-methylphenyl)]methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 1-azabicyclo(2.2.2)octane-4-carboxylate | HCID 573424 | — |
| Reactant | HCID 178425413 | HCID 178425413 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Azabicyclo[2.2.2]oct-4-yl[bis(3-methylphenyl)]methanol | HCID 68962889 | 69.4% |
Reaction Steps
A solution of 3-methylphenylmagnesiumbromide (1.0 M in THF, 3.3 mL, 3.3 mmol) was chilled down to 0° C. under Ar. Ethyl 1-azabicyclo[2.2.2]octane-4-carboxylate (0.1484 g, 0.810 mmol) in THF (4 mL) was slowly added to the reaction mixture at 0° C. over 20 min. The reaction was allowed to warm up to room temperature and then heated at 60° C. for 16 h. The reaction was chilled in an ice bath, quenched with saturated NH4Cl, and concentrated under vacuum. The resulting residue was treated with H2O and extracted with EtOAc. The combined organic layers were dried with MgSO4, filtered, and concentrated under vacuum to yield the desired product (0.1806 g, 69.4%). EI-MS m/z 322 (M+H+) Rt (1.54 min).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309572B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-4de16c29f8194e66a9777183ed92c35e |
| Source note | uspto-grants-2012_11 |