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Isopropanol → 5,7-Dimethyl-imidazo[1,2-f]phenanthridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3,5-Dimethyl-6-phenanthridinamine | HCID 57453549 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5,7-Dimethyl-imidazo[1,2-f]phenanthridine | HCID 58162688 | 40% |
反応手順
3,5-Dimethyl-6-phenanthridinamine (8.6 g, 39 mmol), a 50% solution of acetyl chloride (4.6 g, 58 mmol) in water, sodium bicarbonate (6.5 g, 77.4 mmol) in 258 mL of isopropyl alcohol were heated to reflux for 40 hours. After cooling the crude product was dissolve into methylene chloride and vacuum filtered. The filtrate was concentrated and the crude product was crystallized in methylene chloride and ethyl acetate mixture. The pure product was collected by vacuum filtration to give 5,7-dimethyl-imidazo[1,2-f]phenanthridine) (3.8 g, 40% yield) as determined by NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09281483B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-28335f85ec1747ae9118d04f79440568 |
| 出典メモ | uspto-grants-2016_03 |