化工社化工社 化学情報印刷レポート · 研究参考用
Acetyl chloride → 10-Fluoro-imidazo[1,2-f]phenanthridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 9-Fluoro-6-phenanthridinamine | HCID 11252828 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 10-Fluoro-imidazo[1,2-f]phenanthridine | HCID 58162433 | 52% |
反応手順
9-Fluoro-6-Phenanthridinamine (0.8 g, 3.7 mmol), and a 50% solution of acetyl chloride (0.4 g, 5.66 mmol) in water containing sodium bicarbonate (0.6 g, 7.54 mmol) was dissolved in isopropyl alcohol (25 mL). The reaction mixture was refluxed for 17 hours under a nitrogen pad. The reaction mixture was cooled to room temperature and the precipitate vacuum filtered and washed with methylene chloride. The crude product was purified by column chromatography using a 1:1 ratio of ethyl acetate and hexanes as the eluants followed by distillation to give 10-fluoro-imidazo[1,2-f]phenanthridine) (0.46 g, 52% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889864B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-db6bfb6682ad46a7a5f710fde2221c21 |
| 出典メモ | uspto-grants-2014_11 |