関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | 2,5-Dimethylpiperazine | HCID 7816 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Isoquinolinesulfonyl chloride | HCID 3371655 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(5-Isoquinolinesulfonyl)-2,5-dimethylpiperazine | HCID 13229178 | 59.5% |
反応手順
In 30 ml of methylene chloride were dissolved 1.75 g of 2,5-dimethylpiperazine and 1.53 g of triethylamine, and to the solution was added dropwise 20 ml of a methylene chloride solution containing 1.73 g of 5-isoquinolinesulfonyl chloride under cooling with ice. After the dropwise addition of the methylene chloride solution, the mixed solution obtained was stirred at a temperature of 5° C. to 10° C. for three hours, and then the reaction mixture solution was washed with water and dried with anhydrous magnesium sulfate. After the methylene chloride was distilled therefrom, the residue obtained was subjected to an alumina column chromatography (alumina: 50 g; solvent: chloroform) to give 1.38 g of 1-(5-isoquinolinesulfonyl)-2,5-dimethylpiperazine, Compound (40) in a yield of 59%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04560755 |
|---|
| 出典データセット | uspto-grants-1985_12 |
|---|
| ORD ID | ord-7bd55402f86b43b0b6c675fd34f2c672 |
|---|
| 出典メモ | uspto-grants-1985_12 |
|---|