Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Carbamimidoylazanium Chloride | HCID 5460839 | — |
| Edukt | ethyl (2-methyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate | HCID 10633389 | — |
| Edukt | Potassium tert-butoxide | HCID 23665647 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 178481324 | HCID 178481324 | 16,6% |
Reaktionsschritte
4.3 g of guanidinium chloride are added to a suspension of 5.2 g of potassium tertbutoxide in 100 cm3 of dimethylformamide. The reaction mixture is stirred under an inert atmosphere at a temperature in the region of 20° C. for 1 hour, followed by addition of a solution of 2 g of ethyl (2-methyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate in 20 cm3 of dimethylformamide. The reaction mixture is stirred at a temperature in the region of 20° C. for 16 hours, followed by addition of 100 cm3 of water. The pH is adjusted to 8 by adding 50 cm3 of 1 N hydrochloric acid, and the mixture is concentrated under reduced pressure (0.6 kPa) at a temperature in the region of 30° C. The evaporation residue is taken up in water and then filtered. 0.35 g of N-[(2-methyl3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetyl]guanidine is thus obtained in the form of an off-white solid melting at 214° C. Mass spectrum EI: m/e 246 (M+), m/e 159 (base peak), m/e 146.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07078428B2 |
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| Quelldatensatz | uspto-grants-2006_07 |
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| ORD ID | ord-61d100dc066b46178c90cd89026a6194 |
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| Quellennotiz | uspto-grants-2006_07 |
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