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海萝胶 → HCID 178463795,化合物
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 海萝胶 | HCID 313 | — |
| 反应物 | N,N-二乙基对苯二胺 | HCID 7120 | — |
| 反应物 | 重铬酸钾 | HCID 24502 | — |
| 反应物 | N-[3-(dimethylamino)phenyl]methanesulphonamide | HCID 13796402 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 产物 | HCID 178463795 | HCID 178463795 | 22% |
反应步骤
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%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US08658665B2 |
| 来源数据集 | uspto-grants-2014_02 |
| ORD ID | ord-62fc057aeeea43c299d1f805d62a92e3 |
| 来源说明 | uspto-grants-2014_02 |