化工社化工社 化学情報印刷レポート · 研究参考用
Phosphorus oxychloride → 1H-Indole-3-carboxaldehyde, 1-methyl-2-phenyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 1-Methyl-2-phenylindole | HCID 77095 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1H-Indole-3-carboxaldehyde, 1-methyl-2-phenyl- | HCID 74468 | — |
反応手順
To 150 ml of dimethylformamide 46 ml of phosphorus oxychloride were added dropwise care being taken that the temperature of the reaction mixture did not rise above 20° C. Subsequently to the obtained mixture 103.5 g of 1-methyl-2-phenyl-indole dissolved in 200 ml of dimethylformamide were added dropwise. During the addition the temperature of the reaction mixture was kept in the range of 20° to 40° C and thereupon for 1 hour between 40° and 45° C. Then the reaction mixture was poured into a solution of 490 g of sodium acetate dissolved in 500 ml of water to which 500 g of ice were added. The precipitated aldehyde was separated by suction, washed with water and methanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04008085 |
| 出典データセット | uspto-grants-1977_02 |
| ORD ID | ord-95283ecf5330478b97733e8a59277787 |
| 出典メモ | uspto-grants-1977_02 |