Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Formaldehyde → 1-(4-Chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | p-Chlorothiophenol | HCID 7815 | — |
| 반응물 | Piperidine | HCID 8082 | — |
| 반응물 | 3,3-Dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanone | HCID 100877 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1-(4-Chlorophenylthio)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pentan-3-one | HCID 13191365 | 28% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04699645 |
| 출처 데이터셋 | uspto-grants-1987_10 |
| ORD ID | ord-928c673c32af4ee084ea5f08ee68500e |
| 출처 메모 | uspto-grants-1987_10 |