Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tripropylamine | HCID 7616 | — |
| Reactant | 1-(2-Ethoxyphenyl)piperazine | HCID 83357 | — |
| Reactant | HCID 70192625 | HCID 70192625 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 44213422 | HCID 44213422 | 57% |
Reaction Steps
4.3 g (15 mmol) of 6-(3-chloropropylamino)-5-cyanoethyl-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione and 4.2 g (15 mmol) of 1-(2-ethoxyphenyl)piperazine are heated at 140° C. for 14 h with 11.4 ml (60 mmol) of tripropylamine in 50 ml of xylene. The reaction mixture is concentrated in vacuo, the residue is taken up with 50 ml of water and 200 ml of ethyl acetate, and the mixture is treated with 300 ml of 1N NaOH, extracted and separated. The organic extract is washed with saturated NaCl solution and dried and the oil obtained after removing the solvent is purified by column chromatography (neutral silica gel, eluent initially ethyl acetate/petroleum ether 1:1, later only petroleum ether). The title compound of m.p. 133-136° C. (from ether) is obtained from the product fractions in a yield of 57%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06046329 |
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| Source dataset | uspto-grants-2000_04 |
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| ORD ID | ord-21e9c69855a5417592bfa45bc8eae6da |
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| Source note | uspto-grants-2000_04 |
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