Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Carbonate Ion | HCID 19660 | — |
| Reactant | HCID 68907722 | HCID 68907722 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57635045 | HCID 57635045 | 54.2% |
Reaction Steps
To a suspension of 0.045 g of (rac)-4-(9-cyclohexyl-7-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-N-(1-methyl-piperidin-4-yl)-benzamide trifluoro-acetic acid salt in tetrahydrofuran was added 0.2 g of SilicaBond Carbonate (Silicycle). The mixture was stirred at room temperature for 3 hours, then filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography eluting with dichloromethane-methanol (100:0-75:25) to give 0.020 g of (rac)-4-(9-cyclohexyl-7-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-N-(1-methyl-piperidin-4-yl)-benzamide (I-18) as a white powder. HRMS (ES+) m/z Calcd for C28H39N7O3+H [(M+H)+]: 522.3187. Found: 522.3187.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07517873B2 |
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| Source dataset | uspto-grants-2009_04 |
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| ORD ID | ord-5d425e4da72e48188984099f11585ae2 |
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| Source note | uspto-grants-2009_04 |
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