化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Iodide → 10-(3-diethylamino-propylamino) 5H-pyrido[3',4':4,5]pyrrolo[2,3-g]isoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | Hexamethyldisilazane | HCID 13838 | — |
| 反応物 | N,N-Diethyl-1,3-propanediamine | HCID 61011 | — |
| 反応物 | 10-methoxy 6-methyl 5H-pyrido[3',4':4,5]pyrrolo[2,3-g]isoquinoline | HCID 11021716 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 10-(3-diethylamino-propylamino) 5H-pyrido[3',4':4,5]pyrrolo[2,3-g]isoquinoline | HCID 57067349 | — |
反応手順
0.87 g (0.0033 mole) of 10-methoxy 6-methyl 5H-pyrido[3',4':4,5]pyrrolo[2,3-g]isoquinoline and 0.495 g (0.003 mole) of sodium iodide are suspended in 25 ml of acetonitrile and 4.2 ml (0.33 mole) of trimethylsilylchloride, and then heated at 40° C. for 17 hours. 10.5 ml (0.050 mole) of hexamethyldisilazane, 0.113 g (6×10-4 mole) of anhydrous p-toluenesulfonic acid and 22.4 ml (0.14 mole) of diethylaminopropylamine are then added. After distillation of the acetonitrile, the mixture is heated at reflux for 20 hours. It is evaporated to dryness under a partial vacuum and the residue is stirred with 20 ml of water and 5 ml of diisopropyl ether for 1 hour. The precipitate obtained is filtered off and dried under vacuum at 50° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05079363 |
| 出典データセット | uspto-grants-1992_01 |
| ORD ID | ord-e86c1c5b169b4ebeb61e406073a700ff |
| 出典メモ | uspto-grants-1992_01 |