Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dabco | HCID 9237 | — |
| Reactant | N-Methylethylamine | HCID 12219 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 15462514 | HCID 15462514 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 68007175 | HCID 68007175 | — |
Reaction Steps
To a solution of N-ethylmethylamine (78 mg) and triphosgene (209 mg) in dichloromethane (10 ml) was added dropwise triethylamine (365 μl) at room temperature and the mixture was stirred for 10 minutes. To the reaction mixture was added a solution of 9-methyl-2-phenyl-7,9-dihydro-8H-purine-8-one <the compound of Reference Example 21> (200 mg) and 1,4-diazabicyclo[2.2.2]octane (220 mg) in dichloromethane (10 ml) and the mixture was stirred for 1 hour. The reaction mixture was washed with water and the organic layer was, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=100/0˜0/100) to give the title compound 156 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08735406B2 |
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| Source dataset | uspto-grants-2014_05 |
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| ORD ID | ord-e4199f8b5601441d92d5c365573cacfc |
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| Source note | uspto-grants-2014_05 |
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