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Sodium Chloride → N-4-Chlorocinnamyl-1,2-phenylenediamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | O-Phenylenediamine | HCID 7243 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | p-Chlorocinnamyl chloride | HCID 53728250 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-4-Chlorocinnamyl-1,2-phenylenediamine | HCID 54229126 | 82.2% |
反応手順
19.6 g of 1,2-phenylenediamine was dissolved in 300 ml of dimethylformamide, to the solution were added 11.3 g of the above-prepared 4-chlorocinnamyl chloride crystals and 12.5 g of potassium carbonate at a room temperature with stirring, and the mixture was stirred for 48 hours under the same condition. After adding water and sodium chloride, the reaction mixture was extracted twice with 1000 ml of chloroform, and the extract was dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure. Resulting residue was applied to a silica gel column and eluted with hexane/ethyl acetate (3:1), to obtain 12.85 g of the title compound as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05245034 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-c09855ed64714736b79c8d5024c94a04 |
| 出典メモ | uspto-grants-1993_09 |