Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 2-Isocyanatoethyl methacrylate | HCID 35409 | — |
| Edukt | Dibutyltin oxide | HCID 61221 | — |
| Edukt | HCID 178429414 | HCID 178429414 | — |
| Lösungsmittel | Dimethylacetamide | HCID 31374 | — |
| Produkt | HCID 178454713 | HCID 178454713 | — |
Reaktionsschritte
37.5 g (0.3 mol) 6-methylisocytosine, 55.8 g (0.36 mol) 2-isocyanatoethyl methacrylate and 3.7 g (0.015 mmol) dibutyltin oxide were added to 400 ml dimethylacetamide. 100 mg BHT was added and the mixture was heated to 90° C. for one hour. The mixture was filtered at 90° C. Upon cooling down to room temperature 2-methyl-2-propenoic acid-2-[[[(1,4-dihydro-6-methyl-4-oxo-2-pyrimidinyl)amino]carbonyl]amino]ethyl ester started to crystallize. The mixture was stirred for two and a half hour. 500 ml acetone was added and 3-methyl-2-propenoic acid-2-[[[(1,4-dihydro-6-methyl-4-oxo-2-pyrimidinyl)amino]carbonyl]amino]ethyl ester was isolated by filtration. 2-methyl-2-propenoic acid-2-[[[(1,4-dihydro-6-methyl-4-oxo-2-pyrimidinyl)amino]carbonyl]amino]ethyl ester was treated with 500 ml acetone, again isolated by filtration and dried. 68.6 g (82%) of 2-methyl-2-propenoic acid-2-[[[(1,4-dihydro-6-methyl-4-oxo-2-pyrimidinyl)amino]carbonyl]amino]ethyl ester was isolated (m.p.:208° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08192918B2 |
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| Quelldatensatz | uspto-grants-2012_06 |
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| ORD ID | ord-927182cec925424f8410152396a87b1f |
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| Quellennotiz | uspto-grants-2012_06 |
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