関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(Bromomethyl)-3-chloro-2-fluorobenzene | HCID 522827 | — |
| 反応物 | HCID 178516656 | HCID 178516656 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-[(3-Chloro-2-fluorobenzyl)thio]-4,6-pyrimidinediol | HCID 178516653 | — |
反応手順
To a slurry of 2-mercapto-4,6-pyrimidinediol (64.6 g) in ethanol (387 ml) and H2O (387 ml) was added sodium hydroxide (18 g) in H2O (82 ml) Causing almost a complete solution to form. 2-Fluoro-3-chloro-benzylbromide (100 g) in ethanol (82 ml) was then added dropwise over 30 min causing a thick precipitate to form. Stirring was continued for a further 4 h and the whole then cooled to 0° C. before filtering the white solid formed and then washing with water. The collected solid was dried in vacuo at 50° C. for 48 h leaving the subtitle compound as a white solid. Yield: 125.7 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08106063B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-ec5234dcedbf42319215a712740913bb |
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| 出典メモ | uspto-grants-2012_01 |
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