Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 118024061 | HCID 118024061 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 118023386 | HCID 118023386 | — |
Reaction Steps
To a mixture of 6-(4,4-dimethylcyclohexyl)-4-[(2,2-dimethylpiperazin-1-yl)methyl]-2-methylthieno[2,3-d]pyrimidine (40 mg), pyridine (83 μL), and DCM (1.2 mL) was added acetic anhydride (49 μL), followed by stirring at room temperature for 30 minutes. To the reaction mixture was added water, followed by extraction with EtOAc. The organic layer was washed with brine, dried over MgSO4, and then concentrated under reduced pressure. The residue was purified by silica gel column. To a solution of the obtained purified product in EtOAc was added dropwise 4 M HCl/dioxane, and the precipitate was collected by filtration and dried to obtain 1-(4-{[6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4-yl]methyl}-3,3-dimethylpiperazin-1-yl)ethanone hydrochloride (35 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09051339B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-67114f93963445d8af5bdac2f1341ac3 |
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| Source note | uspto-grants-2015_06 |
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