HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → 1-{4-[4-(2,4-Dichlorobenzyl)piperazin-1-yl]butyl}-5-methyl-1H-pyrimidine-2,4-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | Sodium Bromide | HCID 253881 | — |
| Edukt | 1-(2,4-Dichlorobenzyl)piperazine | HCID 411179 | — |
| Edukt | 1-(4-chlorobutyl)-5-methylpyrimidine-2,4(1H,3H)-dione | HCID 59337587 | — |
| Lösungsmittel | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Produkt | 1-{4-[4-(2,4-Dichlorobenzyl)piperazin-1-yl]butyl}-5-methyl-1H-pyrimidine-2,4-dione | HCID 11718810 | 33,4% |
Reaktionsschritte
1-(4-Chlorobutyl)-5-methyl-1H-pyrimidine-2,4-dione (0.69 mmol, 0.15 g), 1-(2,4-dichlorobenzyl)piperazine (0.62 mmol, 0.15 g), sodium bromide (3.46 mmol, 0.36 g) and diisopropylethylamine (6.92 mmol, 0.89 g) were heated in N-methylpyrrolidinone (0.6 ml) at 120° C. for 5 hours. The reaction mixture was then allowed to cool, the suspension was filtered with suction, and the filtrate was concentrated. The residue was then then taken up in ethyl acetate and washed with saturated brine. The organic layer was dried, filtered to remove the desiccant and evaporated in vacuo. The resulting residue was purified by chromatography on silica gel (eluent: methyl tert-butyl ether/methanol (0-100%), resulting in 88.0 mg of the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08114875B2 |
| Quelldatensatz | uspto-grants-2012_02 |
| ORD ID | ord-85ba6cec0af0423ba4949588bab461f4 |
| Quellennotiz | uspto-grants-2012_02 |