Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Benzhydrylpiperazine | HCID 70048 | — |
| Reactant | HCID 54007979 | HCID 54007979 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 67937927 | HCID 67937927 | 36.1% |
Reaction Steps
A mixture of 1.0 g of N-[3-(6-methyl-3-pyridyl)acryloyl]-3-amino-1-chloropropane, 1.0 g of 1-diphenylmethylpiperazine, 0.55 g of potassium carbonate, 0.55 g of sodium iodide, and 30 ml of methyl ethyl ketone is refluxed with stirring for 6 hours. The reaction mixture is concentrated, and 20 ml of water is added. The mixture is extracted with three 30-ml portions of chloroform. The combined extracts are dried over magnesium sulfate, and the chloroform is distilled off. The residue is chromatographed on silica gel with chloroform-methanol (30:1) to give 0.65 g of the title compound. The product is converted into the fumarate in a usual manner to give the trifumarate 3/4 hydrate of the title compound. m.p. 196°-200° C. (recrystallized from ethanol)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04778796 |
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| Source dataset | uspto-grants-1988_10 |
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| ORD ID | ord-9db3f4582a214d3c904fff26b428ab66 |
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| Source note | uspto-grants-1988_10 |
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