化工社化工社 化学情報印刷レポート · 研究参考用
Water → 2-Bromo-7-nitro-5-trityl-pyrrolo[2,3-b]pyrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-bromo-7-nitro-5H-pyrrolo[2,3-b]pyrazine | HCID 86675704 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Bromo-7-nitro-5-trityl-pyrrolo[2,3-b]pyrazine | HCID 86675706 | — |
反応手順
2-bromo-7-nitro-5H-pyrrolo[2,3-b]pyrazine (5 g, 20.57 mmol) was dissolved in DMF (100 mL) under N2. Solution was cooled in an ice bath and sodium hydride (867.1 mg, 22.63 mmol) added portionwise. After 30 minutes (effervescence completed) trityl chloride (6.022 g, 21.60 mmol) was added in one portion and the mixture allowed to warm to ambient temperature (Precipitate observed after around 15 mins). Reaction mixture was poured into water and mixture stirred for 1 hour then filtered. Solid was washed with copious water then dried in a vacuum oven over 48 hours at 80° C. Taken on to the next step as is. (9.7 g, 97.3%) 1H NMR (400.0 MHz, DMSO) δ 8.46 (s, 1H), 8.40 (s, 1H), 7.38-7.36 (m, H), 7.23-7.20 (m, 8H) and 3.32 (s, 7H) ppm
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822469B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-e05f3a61001a413aa89e62427f7b0093 |
| 出典メモ | uspto-grants-2014_09 |