Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 2-Methylpentanedinitrile | HCID 20686 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3-Methyl-2,6-piperidinedione | HCID 34629 | 67% |
Reaktionsschritte
A solution of H2SO4 (80 ml), acetic acid (500 ml) and 2-methylpentanedinitrile (128.0 g, 1184 mmol) was stirred at room temperature. An aqueous solution of acetic acid (100 ml in 32 ml water) was then added dropwise. Upon completion of the addition, the reaction was heated to 130° C. for 1 hour. The reaction was then allowed to cool to room temperature and filtered to remove solids, which were washed with acetic acid (100 ml). The filtrate was then concentrated until a residue resulted. This residue was poured into water (0.75 l), and adjusted to pH 5 with Na2CO3. The resulting solid was collected by filtration and washed with cold water to give the title compound (101 g, 67%) which was used without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08324252B2 |
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| Quelldatensatz | uspto-grants-2012_12 |
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| ORD ID | ord-262bfbe611734fbe9d1f289a777c9bf1 |
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| Quellennotiz | uspto-grants-2012_12 |
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