化工社化工社 化学情報印刷レポート · 研究参考用
Formaldehyde → 1-(4-Chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | p-Chlorothiophenol | HCID 7815 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 3,3-Dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanone | HCID 100877 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(4-Chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one | HCID 13191365 | 28% |
反応手順
A mixture of 72.5 g (0.5 mol) of 4-chlorothiophenol, 100.2 g (0.6 mol) of 1,2,4-triazol-1-yl-pinacolin, 18 g (0.6 mol) of paraformaldehyde, 15 g of acetic acid and 5 ml of piperidine in 600 ml of toluene was heated under reflux in a water separator. After the water has been separated off, the reaction solution was washed with water, dried over sodium sulphate, filtered, and concentrated in vacuo. The oily residue was chromatographed over a silica gel column (mobile phase: chloroform). 45 g (28% of theory) of 1-(4-chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pentan -3-one of melting point 67° C. were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04699645 |
| 出典データセット | uspto-grants-1987_10 |
| ORD ID | ord-928c673c32af4ee084ea5f08ee68500e |
| 出典メモ | uspto-grants-1987_10 |