HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 44252387, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4-Benzyl-1-(dimethylamino)-4-((dimethylamino)methyl)cyclohexane carbonitrile | HCID 68631452 | — |
| Reactant | HCID 178478979 | HCID 178478979 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 44252387 | HCID 44252387 | — |
Reaction Steps
The title compound of step 1 (0.88 g, 2.94 mmol) was dissolved in THF (35 mL) and mixed in drops with 2M phenylmagnesium chloride solution (5.1 mL, 10.2 mmol) with ice cooling. The reaction solution was heated to boiling for 8 h. For work up the solution was mixed with 20% NH4Cl solution (0.6 mL) and water (0.4 mL) with ice cooling, extracted with ether (3×25 mL), the ether solution was washed with water, dried (Na2SO4) and concentrated to low volume in a vacuum. The residue was purified by column chromatography with EtOH/EE (1:20). 2 fractions were obtained, wherein according to LCMS, inter alia, the more polar fraction (300 mg) contained the desired substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835689B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-d90be85c97b64aca98b76ff78f3f5df4 |
| Source note | uspto-grants-2014_09 |