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Water → 6-(2,4-Dichlorophenyl)-2-(ethylthio)pyrimidine-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione | HCID 58305993 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 6-(2,4-Dichlorophenyl)-2-(ethylthio)pyrimidine-4-amine | HCID 58306005 | — |
反応手順
67.5 g (248 mmol) of 4-amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione and 77.37 g (496.04 mmol) of iodoethane are dissolved in 560 ml of dry DMSO and, at RT, 270 ml of a saturated aqueous sodium bicarbonate solution are slowly added. The mixture is stirred at RT for 5 h and then 440 ml of water are added. The precipitate is filtered off with suction, washed with water and sucked dry. It is stirred twice with 100 ml of isopropanol each time and again filtered off with suction. It is washed once more with petroleum ether and the residue is dried under high vacuum. 50.0 g (67% 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 | US09051323B2 |
| 出典データセット | uspto-grants-2015_06 |
| ORD ID | ord-00ccfb01c6544563b70b06cf24c6caf1 |
| 出典メモ | uspto-grants-2015_06 |