化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Iodide → 1,3-dimethyl-4-nitro-1H-pyrazole-5-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | 5-Chloro-1,3-dimethyl-4-nitro-1H-pyrazole | HCID 279515 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1,3-dimethyl-4-nitro-1H-pyrazole-5-carbonitrile | HCID 96507 | — |
反応手順
Fifty-five g of 1,3-dimethyl-4-nitro-5-chloropyrazole was dissolved in 400 ml acetonitrile and 17.45 g potassium cyanide added, followed by 0.5 g potassium iodide and 5 ml DMF. The mixture was refluxed for 22 hours, then cooled, and filtered. The filtrate was concentrated under reduced pressure, then added to stirred water. The resulting percipitate was collected, dried, and recyrstallized in isopropanol. mp, 85°-87° C. A second recrystallization again in ethanol gave the product having increased purity, mp 96°-98° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04666908 |
| 出典データセット | uspto-grants-1987_05 |
| ORD ID | ord-02e5eba2d86747a6ad61fc9c271d97c8 |
| 出典メモ | uspto-grants-1987_05 |