HuagongsheHuagongshe Chemistry Print Report · For research reference only
Magnesium → HCID 131732178, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Magnesium | HCID 5462224 | — |
| Reactant | HCID 86722950 | HCID 86722950 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 131732178 | HCID 131732178 | 91.5% |
Reaction Steps
To a solution of Ethyl 2-[(trans)-3,4-bis(dibenzylcarbamoyl)cyclohexylidene]acetate (9.27 g, 15 mmol) in dry MeOH (75 mL) is added Magnesium ribbon (1.08 g, 45 mmol). The suspension was stirred for 5 hr. To this homogeneous solution is added a further batch of Magnesium ribbon (200 mg, 8.2 mmol). This mixture is stirred for 17 hr. The resulting solution is extracted with EtOAc, washed with brine, dried over MgSO4 and concentrated. The residue is purified by silica chromatography (eluting with 20% ethyl acetate/10% dichloromethane in hexane) to give the title compound (8.27 g) as a foam. ESI-MS (m/z) 617 (MH)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08912169B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-b51c33165a8f45b3ba68ff06bab96367 |
| Source note | uspto-grants-2014_12 |