Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Tin tetrachloride | HCID 24287 | — |
| Edukt | Allyl-(3-nitropyridin-4-yl)amine | HCID 23070628 | — |
| Produkt | HCID 57642851 | HCID 57642851 | 93% |
Reaktionsschritte
55 ml of 35% hydrochloric acid was added to 3.02 g of allyl-(3-nitropyridin-4-yl)amine, and the mixture was heated to 90° C. 19.1 g of tin chloride was added to the solution, and the mixture was kept at 90° C. for 30 minutes. The reaction solution was cooled in an ice-water bath, and then 250 ml ice/water was added thereto. The reaction solution was concentrated under reduced pressure, and then 250 ml of ammonia-saturated methanol was added thereto. The mixture was stirred for 20 hours. 750 ml of ethyl acetate was added to the solution, and the mixture was filtered through celite. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography. Thus, 2.88 g of the title compound was obtained from the fraction eluted with ethyl acetate-hexane (1:1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07772226B2 |
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| Quelldatensatz | uspto-grants-2010_08 |
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| ORD ID | ord-9c13a56b5ba44ea2b61999d2929b8fb9 |
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| Quellennotiz | uspto-grants-2010_08 |
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