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Sodium Carbonate → N,N-Diethyl-N'-[2-(phenylsulfinyl)ethyl]-1,2-ethanediamine maleate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | N,N-Diethylethylenediamine | HCID 60993 | — |
| 反応物 | ((2-Chloroethyl)sulphinyl)benzene | HCID 99293 | — |
| 反応物 | Maleic Acid | HCID 444266 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N,N-Diethyl-N'-[2-(phenylsulfinyl)ethyl]-1,2-ethanediamine maleate | HCID 70361008 | 50.3% |
反応手順
A mixture of 20.0 g (0.106 mole) of [(2-chloroethyl)sulfinyl]benzene, 30.0 g (0.259 mole) of N,N-diethylethylenediamine and excess sodium carbonate in 600 ml of acetonitrile was refluxed for 16 hr. The reaction mixture solution was filtered, and the solvent was removed in vacuo. The residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over sodium sulfate and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, and a solution of 2 equivalents of maleic acid in methanol was added. Diethyl ether was added and a whie solid precipitated to give 26.7 g (50.3%) of title compound, a white crystalline solid, mp 111°-112.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04895840 |
| 出典データセット | uspto-grants-1990_01 |
| ORD ID | ord-78f46fb1e0ea463099ce75c3e46f1862 |
| 出典メモ | uspto-grants-1990_01 |