関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(5-Isoquinolinylsulfonyl)piperazine | HCID 3545 | — |
| 反応物 | Ethyl Bromide | HCID 6332 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Chloroform methanol | HCID 21584188 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 13116936 | HCID 13116936 | 74.1% |
反応手順
In 100 ml of ethanol were added 2.77 g of 1-(5-isoquinolinesulfonyl)piperazine, i.e., Compound (35), 1.66 g of anhydrous potassium carbonate and 5.45 g of ethyl bromide, and the reaction was carried out at an external temperature of 70° C. for 24 hours. After the reaction solution was filtered, the filtrate was condensed and the residue was dissolved in 50 ml of chloroform, and the solution was extracted twice with a 2N aqueous hydrochloric acid solution. The aqueous hydrochloric acid layer was rendered alkaline, extracted twice with 50 ml of chloroform, and the chloroform layer extracted was washed with water and dried with anhydrous magnesium sulfate. After the chloroform was distilled therefrom, the residue obtained was subjected to a silica gel column chromatography (silica gel: 100 g; solvent: 2% methanol-chloroform) to give 2.26 g of 1-(5-isoquinolinesulfonyl)-4-ethylpiperazine, i.e., Compound (42) in a yield of 74%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04560755 |
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| 出典データセット | uspto-grants-1985_12 |
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| ORD ID | ord-118dcab10db243cba38965d8a598788b |
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| 出典メモ | uspto-grants-1985_12 |
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