Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 4-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Thiourea | HCID 2723790 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 반응물 | 3-Amino-3-(2,4-dichlorophenyl)acrylonitrile | HCID 66911322 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione | HCID 58305993 | — |
반응 단계
16.51 g (718.08 mmol) of sodium are dissolved in 353 ml of ethanol, and 40.996 g (538.56 mmol) of thiourea are added to the sodium ethanolate solution prepared in this way, followed by 76.5 g (359.04 mmol) of 3-amino-3-(2,4-dichlorophenyl)acrylonitrile. The mixture is heated under reflux for 18 h and, after cooling, 500 ml of water are added. The mixture is neutralized with 1M hydrochloric acid, and the precipitate which has separated out is filtered off with suction. The latter is washed with water, suspended in THF and again filtered off with suction. It is washed with 300 ml of petroleum ether and then dried under high vacuum. 67.5 g (55% of theory) of the product are obtained as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08273752B2 |
| 출처 데이터셋 | uspto-grants-2012_09 |
| ORD ID | ord-3c86153c3d3f4ce798dc081fdc1e4033 |
| 출처 메모 | uspto-grants-2012_09 |