Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Formaldehyde | HCID 712 | — |
| Edukt | Dimethylamine, hydrochloride | HCID 10473 | — |
| Edukt | 3'-Hydroxypropiophenone | HCID 83141 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Isopropanol | HCID 3776 | — |
| Produkt | HCID 56926625 | HCID 56926625 | 55,5% |
Reaktionsschritte
A mixture of 1-(3-hydroxy-phenyl)-propan-1-one (5 g, 0.03 mol), paraformaldehyde (1 g, 0.03 mol), dimethylamine hydrochloride (3 g, 0.04 mol), hydrochloric acid (3.4 ml, 30%) and isopropanol (15 ml) was refluxed for 16 hours. Isopropanol was distilled off from the reaction mixture and resulting reaction mass was cooled to 25-30° C. Water (15 ml) was added to the reaction mass and washed with isopropyl ether (2×15 ml). Layers were separated and aqueous layer was added to a stirred mixture of aqueous sodium hydroxide solution (1.2 g in 16 ml water) and methyl tert-butyl ether (25 ml). Layers were separated. Organic layer was washed with water (10 ml), dried and solvent was distilled to give 3.45 g of the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08552219B2 |
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| Quelldatensatz | uspto-grants-2013_10 |
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| ORD ID | ord-90bebda661f9416ab7c930a73907b21f |
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| Quellennotiz | uspto-grants-2013_10 |
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