化工社化工社 化学情報印刷レポート · 研究参考用
Hydrogen Peroxide → 9H-Indeno[1,2-b]pyrazine-2,3,9(1H,4H)-trione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione | HCID 19035976 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 9H-Indeno[1,2-b]pyrazine-2,3,9(1H,4H)-trione | HCID 19035977 | 79.6% |
反応手順
9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione (20 g, 100.9 mmol), recrystallized from acetic acid, was suspended in a mixture of 135 ml acetic acid and 135 ml acetic anhydride and hydrogen peroxide (9.8 ml, 35%) was added. After stirring overnight another portion (9.8 ml, 35%) of hydrogen peroxide was added. This was repeated five times over a week. The red precipitate was filtered off, washed with acetic acid and water and dried to give 18.5 g (79.6%) of the title compound, which could be further purified by dissolving in aqueous sodium hydroxide and precipitation by hydrochloric acid. M.p. >300° C. 1H-NMR (DMSO-d6, δ): 7.15-7.45 (m, 4H), 12 (s, 1H), 12.8 (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-971dcb27339942aba522e1e9dfeadbe7 |
| 出典メモ | uspto-grants-1995_11 |