化工社化工社 化学情報印刷レポート · 研究参考用
1-Methylpiperazine → 3,4-Bis(4-methylpiperazin-1-yl)cyclobut-3-ene-1,2-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | 3-Cyclobutene-1,2-dione, 3,4-dimethoxy- | HCID 123227 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3,4-Bis(4-methylpiperazin-1-yl)cyclobut-3-ene-1,2-dione | HCID 21423024 | — |
反応手順
A solution of 1.0 gram of 3,4-dimethoxy-3-cyclobutene-1,2-dione dissolved in 30 ml. of absolute ethanol is mixed with a solution of 1.4 grams of 1-methylpiperazine in 30 ml. of absolute ethanol. The resulting mixture is stirred and heated to reflux for 5 hours under an atmosphere of dry nitrogen. After concentration to approximately one-sixth the volume under reduced pressure, the reaction mixture is cooled and crystallization is induced by scratching. The resultant precipitate is filtered, washed with 0.5 ml. of absolute ethanol, and dried in a steam cabinet. The resulting, product, 3,4-bis(4-methyl-1-piperazinyl)-3-cyclobutene-1,2-dione is obtained as white crystals melting at about 189°-191° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04036828 |
| 出典データセット | uspto-grants-1977_07 |
| ORD ID | ord-7410d28cffb0491395fb23b9c4298dfe |
| 出典メモ | uspto-grants-1977_07 |