HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 9H-Indeno[1,2-b]pyrazine-2,3,9(1H, 4H)-trione 9-ethylene dithioacetal
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Boron trifluoride etherate | HCID 8000 | — |
| Edukt | 1,2-Ethanedithiol | HCID 10902 | — |
| Edukt | 9H-Indeno[1,2-b]pyrazine-2,3,9(1H,4H)-trione | HCID 19035977 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 9H-Indeno[1,2-b]pyrazine-2,3,9(1H, 4H)-trione 9-ethylene dithioacetal | HCID 86749111 | 83% |
Reaktionsschritte
A suspension of 9H-indeno[1,2-b]pyrazine-2,3,9(1H, 4H)-trione. 0.9 H2O (2.0 g, 8.68 mmol) in toluene (50 ml), 1,2-ethanedithiol (2.19 ml, 26.04 mmol) and boron trifluoride etherate (1.07 ml, 8.68 mmol) was refluxed for 20 hours. The reaction mixture was cooled to room temperature, and the precipitate was filtered off and washed with toluene, ethanol-water (2:1) and ethanol. The crude material (2.40 g) was recrystallized from DMF-water to give 2.09 g (83%) of the title compound. M.p. >300° C. 1H-NMR (DMSO-d6, δ): 3.68 (m, 2H), 3.91 (m, 2H), 7.2 (t, 1H), 7.3 (t, 1H), 7.51 (d, 1H), 7.59 (d, 1H), 12.05 (s, 1H), 12.38 (s, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05468748 |
| Quelldatensatz | uspto-grants-1995_11 |
| ORD ID | ord-e3791f7b9e7e4eae98cbd9f962e98b24 |
| Quellennotiz | uspto-grants-1995_11 |