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Phosphorus oxychloride → 6-chloro-3,5-dibenzylpyrimidine-2,4(1H,3H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 3,5-dibenzylpyrimidine-2,4,6(1H,3H)-trione | HCID 268731 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-chloro-3,5-dibenzylpyrimidine-2,4(1H,3H)-dione | HCID 18936661 | — |
反応手順
To 16.8 ml of 50% ethanol, 78.7 ml (844 mmol) of phosphorus oxychloride was added drop by drop, with stirring under ice cooling conditions. To this solution, 30.83 g (100 mmol) of 3,5-dibenzylpyrimidine-2,4,6(1H,3H)-trione was added little by little. This mixture was stirred at 50° C. for 30 minutes and then at 100° C. for 90 minutes. After cooling, the reaction mixture was poured into ice water and stirred for 1 hour. The resulting precipitate was collected by filtration, washed with water and n-hexane and dried to yield 32.62 g (99.8%, light white crystal) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05840732 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-95574b1b83ac4a4db004997c82ad10ad |
| 出典メモ | uspto-grants-1998_11 |