Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium formate | HCID 2723923 | — |
| Reactant | HCID 59312305 | HCID 59312305 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 25070581 | HCID 25070581 | 85% |
Reaction Steps
Under nitrogen, a mixture of 7-benzyl-4-chloro-2-(4-methylbenzyl)-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine of Preparation 35, Step B, (150 mg, 0.40 mmol), ammonium formate (250 mg, 4.0 mmol) and 20% palladium on charcoal (15 mg) in ethanol (5 ml) was heated at 75° C. for 1 h. After returning to room temperature, the mixture was filtered through a pad of Arbocel, washing the pad with ethanol. The combined eluates were concentrated in vacuo and the residue purified by column chromatography on silica gel, eluting with dichloromethane:methanol:0.880NH3, 95:5:0.5 then 90:10:1, to afford the title compound as an oil in 85% yield, 85 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07928099B2 |
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| Source dataset | uspto-grants-2011_04 |
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| ORD ID | ord-af0c7f8b432e46fba43deac7385c3928 |
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| Source note | uspto-grants-2011_04 |
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