関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | HCID 178419104 | HCID 178419104 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Chloro-6-methyl-2-(propan-2-yl)pyrimidine | HCID 3306907 | — |
反応手順
76.1 g of 2-isopropyl-6-methyl-4-pyrimidinol [2814-20-2] (500 mmol) are dissolved in 300 ml of toluene at 90° C. 80.5 g of phosphorus oxychloride (525 mmol) are added dropwise thereto at from 90 to 103° C., and the reaction mixture is heated at 110° C. for 2 hours. After cooling to 20° C., the reaction mixture is adjusted to pH 8 using 4M sodium hydroxide solution, with cooling. The aqueous phase is separated off and extracted with 100 ml of toluene. The combined organic phases are washed three times with 100 ml of water each time and dried at RT under 2 mbar. 89.7 g (105%; contains toluene) are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07731985B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-c1733baf1fbe4d7cba07485c4f3375fa |
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| 出典メモ | uspto-grants-2010_06 |
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