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Hydrochloric Acid → 4-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 3-Amino-3-(2,4-dichlorophenyl)acrylonitrile | HCID 66911322 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione | HCID 58305993 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08273752B2 |
| 出典データセット | uspto-grants-2012_09 |
| ORD ID | ord-3c86153c3d3f4ce798dc081fdc1e4033 |
| 出典メモ | uspto-grants-2012_09 |