Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Edukt | (9aR)-octahydro-1H-pyrido(1,2-a)pyrazine-1,4-dione | HCID 66936119 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | (R)-Octahydro-pyrido[1,2-a]pyrazine | HCID 773775 | 69,5% |
Reaktionsschritte
(R)-Octahydro-1,4-dioxo-2H-pyrido[1,2-a]pyrazine (0.5 g, 2.98 mmol) was added portionwise to a stirred solution of lithium aluminium hydride (1M in tetrahydrofuran; 11.9 ml, 11.9 mmol). The resulting mixture was heated under reflux for 0.5 h. The solution was then cooled to 0° C. and treated dropwise with water (1.35 ml), 1 M sodium hydroxide solution (0.45 ml), then water (1.35 ml). Tetrahydrofuran (10 ml) was added and the solution stirred for 0.5 h, before filtration. The filter cake was washed with tetrahydrofuran (2×5 ml) and the combined filtrate and washings concentrated to yield (R)-octahydro-2H-pyrido[1,2-a]pyrazine as a yellow oil (0.29 g, 2.07 mmol).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07304064B2 |
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| Quelldatensatz | uspto-grants-2007_12 |
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| ORD ID | ord-d8177b0d07644d80a3a48c4387a17559 |
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| Quellennotiz | uspto-grants-2007_12 |
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