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Boron trifluoride etherate → 9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione 9-ethylene dithioacetal
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | 1,2-Ethanedithiol | HCID 10902 | — |
| 反応物 | 9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione | HCID 19035976 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione 9-ethylene dithioacetal | HCID 86749110 | 64% |
反応手順
A suspension of 9H-indeno[1,2-b]pyrazine-3,9(4H)-dione (0.50 g, 2.52 mmol) in benzene (10 ml), 1,2-ethanedithiol (0.63 ml, 7.56 mmol) and boron trifluoride etherate (0.31 ml, 2.52 mmol) was refluxed for 23 hours. The reaction mixture was cooled to room temperature, and the precipitate was filtered off and washed with benzene and water and dried. The crude material (0.64 g) was recrystallized twice from ethanol to give 0.44 g (64%) of the title compound. M.p. 284°-290° C. 1H-NMR (DMSO-d6, δ): 3.75-3.94 (m, 4H), 7.46-7.57 (m, 2H), 7.8 (m, 2H), 7.95 (s, 1H), 12.6 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05468748 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-c086d65008a8409bb356937ba2a25f87 |
| 出典メモ | uspto-grants-1995_11 |