関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(2-Methoxyphenyl)piperazine | HCID 1346 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (2-Bromoethyl)tritylamine | HCID 15718287 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-[4-(2-Methoxyphenyl)piperazin-1-yl]-N-(triphenylmethyl)ethanamine | HCID 15718288 | 70.9% |
反応手順
10 g (0.273 mol) of 2-bromo-N-(triphenylmethyl)ethanamine, 200 ml of acetonitrile, 5.15 g (0.0273 mol) of 1-(2-methoxyphenyl)piperazine, 5.6 g of anhydrous potassium carbonate, a few grains of sodium iodide and 1 ml of dimethylformamide are introduced into a 500 ml round-bottomed flask equipped with a reflux condenser and placed under nitrogen. The mixture is heated at reflux for 15 h, the solvents are evaporated, water and dichloromethane are added, the organic phase is separated, washed with water, dried over sodium sulphate and the solvent is evaporated under reduced pressure. A viscous oil is obtained which is purified by chromatography on a column of silica gel, the eluent being a mixture of ethyl acetate and dichloromethane. There are isolated 9.24 g of product which is used as is in the following stage.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05420130 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-4daa1fcf7cfe48e6859b359d484a1e7b |
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| 出典メモ | uspto-grants-1995_05 |
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