HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 25070908, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | 1-Methyl-1,4-cyclohexadiene | HCID 78006 | — |
| Reactant | HCID 59312363 | HCID 59312363 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Product | HCID 25070908 | HCID 25070908 | 69% |
Reaction Steps
Palladium hydroxide (20% on carbon) (43 mg, 0.3 mmol) and 1-methyl-1,4-cyclohexadiene (3.42 ml, 30.5 mmol) was added to a solution of 7-benzyl-4-chloro-2-(1-phenylethyl)-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine of preparation 30, Step B, (1.15 g, 3.04 mmol) in ethanol (30 ml) and refluxed, under nitrogen, for 16 h. The reaction mixture was filtered through Arbocel then the filtrate was concentrated in vacuo. The residue was purified by column chromatography on Biotage 40S cartridge, eluting with DCM:MeOH (100:0 to 90:10), to afford the title compound as a solid in 69% yield, 629 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928099B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-a162dfa0a3db45ee944a1830c6763750 |
| Source note | uspto-grants-2011_04 |