Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1-(3-((6-Chloro-2-naphthyl)sulfonyl)propionyl)piperazine | HCID 23130883 | — |
| Edukt | HCID 178482537 | HCID 178482537 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 178482540 | HCID 178482540 | 121,4% |
Reaktionsschritte
A suspension of 1-(3-((6-chloro-2-naphthyl)sulfonyl)propionyl)piperazine (2.5 g) obtained in Example 3a), N-((2Z)-4-chloromethyl-3-methyl-1,3-thiazol-2(3H)-ylidene)-N-methylamine hydrochloride (2.2 g) and potassium carbonate (2.4 g) in DMF (50 mL) was mixed at 65° C. for 3 hours. The solvent was distilled off under reduced pressure, the residue was diluted with an aqueous potassium carbonate solution, and extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The product, which was obtained by the purification of the residue with a basic silica gel column, was dissolved in ethyl acetate. A solution of hydrogen chloride in ether was added thereto, and the mixture was concentrated and dried to give the title compound (2.4 g) as a colorless powder.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07534887B2 |
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| Quelldatensatz | uspto-grants-2009_05 |
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| ORD ID | ord-3a3fbf0254c84df7ae80a04ae775c56e |
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| Quellennotiz | uspto-grants-2009_05 |
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