化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dibromoethane → 1-(4-Chlorocinnamyl)-4-(5-isoquinolinesulfonyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-[2-(4-Chlorocinnamylamino)ethyl]-5-isoquinolinesulfonamide | HCID 176156 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-Chlorocinnamyl)-4-(5-isoquinolinesulfonyl)piperazine | HCID 54203703 | 25.5% |
反応手順
1.31 g of the product of Example 172 was dissolved in 3 ml of dimethylformamide, to the solution were added 644 mg of 1,2-dibromoethane and 1.13 g of anhydrous potassium carbonate at a room temperature, and the mixture was stirred for 24 hours. After adding 100 ml of ethyl acetate, the ethyl acetate layer was sequentially washed with water and a saturated sodium chloride aqueous solution twice in each case, and dried over magnesium sulfate. The solution was filtered and evaporated under a reduced pressure, and resulting residue was purified on a silica gel column (silica gel 50 g, eluant: 5% methanol in chloroform), to obtain 356 mg of the title compound in a colorless amorphous form, while recovering the residual starting material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05245034 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-57a90189c8764512903a44bb9d37a3a5 |
| 出典メモ | uspto-grants-1993_09 |