Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 4(3H)-Pyrimidinone, 2-chloro-3-methyl-6-(4-pyridinyl)- | HCID 11276081 | — |
| Reactant | HCID 67117387 | HCID 67117387 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 53628942 | HCID 53628942 | 187.2% |
Reaction Steps
A solution of 2-(4-chlorophenyl)-6,6-dimethyl-piperazine hydrochloride (155 mg, 0.52 mmol), 2-chloro-3-methyl-6-(4-pyridyl)-pyrimidine-4-one (111 mg, 0.50 mmol) and triethylamine (0.42 mL, 2.50 mmol) in tetrahydrofuran (5 mL) was stirred at room temperature for 6 h. The whole was evaporated in vacuo and the residue was extracted with dichloromethane. The organic layer was washed with water, dried and concentrated in vacuo. The residue was dissolved in methanol (5 mL) and treated with 4M hydrogen chloride in ethyl acetate (0.50 mL, 2.0 mmol) for 20 min. After removing the solvent, filtrating and washing the precipitate with ethanol gave 2-(2-(4-chlorophenyl)-6,6-dimethyl-piperazin-4-yl)-3-methyl-6-pyridin-4-yl-3H-pyrimidin-4-one dihydrochloride (235 mg, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07504411B2 |
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| Source dataset | uspto-grants-2009_03 |
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| ORD ID | ord-4b6569ce1e9846a4b5c75f5aa63335d8 |
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| Source note | uspto-grants-2009_03 |
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