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Hydrochloric Acid → 9-Hydroxy-9H-indeno[1,2-b]pyrazine-2,3(1H,4H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 9H-Indeno[1,2-b]pyrazine-2,3,9(1H,4H)-trione | HCID 19035977 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 9-Hydroxy-9H-indeno[1,2-b]pyrazine-2,3(1H,4H)-dione | HCID 19035985 | 91% |
反応手順
To a stirred suspension of 9H-indeno[1,2-b]pyrazine-2,3,9(1H,4H)-trione. 1H2O (5.0 g, 21.5 mmol) in 200 ml of ethanol and 30 ml of water was added sodium borohydride (1.76 g, 46.5 mmol) in four portions over 2 hours, then 200 ml of water was added and the mixture was stirred for 18 hours at room temperature. The reaction mixture was acidified with hydrochloric acid (70 ml, 1N) to pH 1.5 and the precipitate was filtered off, washed with water and dried to give 4.59 g (91%) of the title compound. M.p. >300° C. 1H-NMR (DMSO-d6, δ): 5.1 (d, 1H), 5.72 (d, 1H), 7.15 (t, 1H), 7.28 (t, 1H), 7.41 (d, 1H), 7.48 (d, 1H), 12.0 (s, 1H), 12.25 (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-c41c5b63054b47528ee23fd73a0170d4 |
| 出典メモ | uspto-grants-1995_11 |