Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Methanol | HCID 887 | — |
| Edukt | Hydroxyurea | HCID 3657 | — |
| Edukt | 1,1-Dimethoxypentan-3-one | HCID 11182677 | — |
| Produkt | HCID 178436837 | HCID 178436837 | — |
Reaktionsschritte
0.388 mol (25.9 g) hydroxy urea were dissolved in 195 ml 2 M HCl, 80 ml of methanol were added and 0.388 mol (56.7 g) of 1,1-dimethoxypentane-3-on (62% content in product mixture) were added dropwise under cooling with the internal temperature being maintained at −6 to −7° C. The solution was thawed to room temperature in an ice bath and stirred for 1 h, then evaporated until dryness. The residue was suspended with 100 ml of acetone, the mixture was cooled to below 0° C. in an ice/ethanol bath, the solid filtered off and washed with little ice-cold acetone. After drying 32.6 g crude product were obtained. The crude product was heated until boiling with 200 ml ethanol, hot filtered and slowly cooled to −18° C. The precipitated solid was filtered off, washed with a little amount of ethanol and dried. 11.7 g of the title compound were obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09422247B2 |
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| Quelldatensatz | uspto-grants-2016_08 |
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| ORD ID | ord-dcb726fdc3bb4008bcf77046605c0b12 |
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| Quellennotiz | uspto-grants-2016_08 |
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