Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Phenylpiperidine | HCID 20038 | — |
| Reactant | 2,4,6-Trichloropyrimidine | HCID 77378 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 58320457 | HCID 58320457 | 34% |
Reaction Steps
The synthesis method shall be explained concretely following the order below. 2,4,6-trichloropyrimidine (20 ml, 165 mmol) and triethylamine (27.7 ml) were dissolved in ether (200 ml), and phenylpiperadine (25.2 ml, 165 mmol) was added under ice cooling. After approximately 1 hour of agitation at room temperature, water was added, and extraction was carried out 2 times with ether. After washing the ether layer with saturated saline, drying was done with MgSO4, and the solvent was distilled away under reduced pressure. Purification was done by silica gel chromatography (hexane:ethyl acetate=19:1), and 17.6 g (34% yield) of 4,6-dichloro-2-(4-phenylpiperazin-1-yl)pyrimidine was obtained. NMR data for the obtained 4,6-dichloro-2-(4-phenylpiperazin-1-yl)pyrimidine is shown below.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08563715B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-3ccf90dc4fe54b9a98ca512a67d82664 |
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| Source note | uspto-grants-2013_10 |
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