Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Dimethyl methoxymalonate | HCID 78718 | — |
| Edukt | Sodium ethoxide | HCID 2723922 | — |
| Edukt | Methanimidamide, hydrochloride (1:1) | HCID 10313058 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 178493933 | HCID 178493933 | — |
Reaktionsschritte
5 g (6.2 mmoles) of formamidine hydrochloride is added at 0° C. and in small quantities into a single-necked flask containing 30 ml of absolute ethanol and 90 ml of a solution of sodium ethylate at a concentration of 1.7 mol/l in ethanol. Stirring is maintained at ambient temperature for about twenty minutes, then 8.5 ml of dimethyl methoxymalonate is added dropwise. Stirring is maintained for 16 hours. The reaction mixture is then acidified with pure acetic acid to a pH between 4 and 5, then concentrated to dryness in the presence of cyclohexane. After impasting the crude product obtained is chromatographed on silicagel eluting with a mixture of methylene chloride-methanol (85-15)and 2% water-acetic acid (1-1). 9.5 g of the expected product is obtained containing a small quantity of sodium acetate salts.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07582640B2 |
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| Quelldatensatz | uspto-grants-2009_09 |
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| ORD ID | ord-c196fe37c24c46fa8843bc802cc48135 |
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| Quellennotiz | uspto-grants-2009_09 |
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