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Hydrochloric Acid → HCID 178463795、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | N,N-Diethyl-p-phenylenediamine | HCID 7120 | — |
| 反応物 | Potassium Dichromate | HCID 24502 | — |
| 反応物 | N-[3-(dimethylamino)phenyl]methanesulphonamide | HCID 13796402 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178463795 | HCID 178463795 | 22% |
反応手順
N,N-diethyl-1,4-phenylenediamine (1.00 g, 6.17 mmol) was added slowly to dilute HCl (700 μl, 32%) in H2O (100 cm3). The mixture was stirred until it was homogeneous. N-[3-(dimethylamino)phenyl]methanesulphonamide (1.32 g, 6.17 mmol) in methanol (60 cm3) was added, followed by a saturated aqueous solution of potassium dichromate (2 cm3). The mixture refluxed for 15 min. The mixture was cooled and diluted with water (200 cm3), acidified with hydrochloric acid (1M) and then extracted with chloroform (6×30 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:9 methanol/dichloromethane) gave the target material as a green solid (451 mg, 22%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08658665B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-62fc057aeeea43c299d1f805d62a92e3 |
| 出典メモ | uspto-grants-2014_02 |