HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 9-(2-Methoxyethoxy)-9H-indeno[1,2-b]pyrazine-2,3(1H, 4H)-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | p-Toluenesulfonic acid | HCID 6101 | — |
| Edukt | 2-Methoxyethanol | HCID 8019 | — |
| Edukt | 9-Hydroxy-9H-indeno[1,2-b]pyrazine-2,3(1H,4H)-dione | HCID 19035985 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Produkt | 9-(2-Methoxyethoxy)-9H-indeno[1,2-b]pyrazine-2,3(1H, 4H)-dione | HCID 23194057 | 60% |
Reaktionsschritte
A suspension of 9-hydroxy-9H-indeno[1,2-b]pyrazine-2,3(1H, 4H)-dione. 1H2O (0.50 g, 2.13 mmol) in benzene (20 ml), 2-methoxyethanol (10 ml) and p-toluensulfonic acid (20 mg) was refluxed with water separation for 20 hours. The reaction mixture was evaporated in vacuo to dryness, the residue was suspended in ethanol (10 ml) and the precipitate was filtered off and washed with ethanol and dried to give 0.48 g of the crude product, which was recrystallized from ethanol to yield 0.35 g (60%) of the title compound. M.p. >300° C. 1H-NMR (DMSO-d6, δ): 3.22 (s, 3H), 3.27-3.51 (m, 4H), 5.24 (s, 1H), 7.18 (t, 1H), 7.33 (t, 1H), 7.42 (d, 1H), 7.5 (d, 1H), 2.06 (s, 1H), 12.29 (s, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05468748 |
| Quelldatensatz | uspto-grants-1995_11 |
| ORD ID | ord-8bf8ea965d464656810ab095eddd73d9 |
| Quellennotiz | uspto-grants-1995_11 |