Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Acetylacetone | HCID 31261 | — |
| Edukt | Morpholine-4-carboximidamide Hydrobromide | HCID 2806564 | — |
| Produkt | 4-(4,6-Dimethylpyrimidin-2-yl)morpholine | HCID 676802 | 90% |
Reaktionsschritte
To a suspension of morpholinoformamidine hydrobromide (2.0 g, 9.52 mmol) in ethanol (6 ml) potassium tert-butoxide (1.068 g, 9.52 mmol) then acetylacetone (2 ml, 20 mmol) were added. The reaction mixture was flashed with argon, sealed in the Emrys process vial and heated under microwave irradiation at 140° C. for 5 min. After cooling it was quenched with ethyl acetate (50 ml), filtered via plug of SiO2 (5 g) and eluted with ethyl acetate. Volatiles were removed in vacuo at 70° C. to furnish 1.65 g of pale brown oil that solidified overnight. Yield 90%. LC-MS (m/z) 193.9 (MH+); tR=0.71. 1H NMR (500 MHz, DMSO-d6): 2.23 (s, 6H), 3.62 (m, 4H), 3.67 (m, 4H), 6.44 (s, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07683058B2 |
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| Quelldatensatz | uspto-grants-2010_03 |
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| ORD ID | ord-93561c729c284735bcad2c693e0a3499 |
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| Quellennotiz | uspto-grants-2010_03 |
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