関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Isoquinolinesulfonyl chloride | HCID 3371655 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(5-Isoquinolinylsulfonyl)piperazine | HCID 3545 | 89% |
反応手順
In 100 ml of methylene chloride were added 6.0 g of piperazine and 1.2 g of anhydrous potassium carbonate, and to the mixture was added dropwise 30 ml of a methylene chloride solution containing 2.0 g of 5-isoquinolinesulfonyl chloride under cooling with ice. After the dropwise addition of the methylene chloride solution, the mixed solution was stirred at a temperature of 15° C. to 25° C. for 15 hours, and then the reaction solution was washed with water, dried with anhydrous magnesium sulfate, and the methylene chloride was distilled therefrom. The residue thus obtained was subjected to a silica gel column chromatography (silica gel: 70 g; solvent: chloroform) to give 2.14 g of 1-(5-isoquinolinesulfonyl)piperazine, i.e., Compound (35) in a yield of 89%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04525589 |
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| 出典データセット | uspto-grants-1985_06 |
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| ORD ID | ord-eb6b8e0254904c0ab13fab875cb741cf |
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| 出典メモ | uspto-grants-1985_06 |
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