関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Fluorophenol | HCID 9743 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,5-Trifluoropyrimidine | HCID 12797307 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5,6-Difluoro-(3-fluorophenoxy)-pyrimidine | HCID 23443922 | — |
反応手順
11.38 g (0.085 mol) of trifluoropyrimidine are dissolved in 240 ml of acetonitrile and admixed with 15.26 g (0.11 mol) of potassium carbonate, and the mixture is cooled to 10° C. Under argon, a solution of 9.52 g (0.085 mol) of 3-fluorophenol in 80 ml of acetonitrile is added dropwise. The mixture is then stirred under argon, without further cooling, for another 18 hours. The mixture is poured into 1 litre of water and extracted three times with in each case 150 ml of ethyl acetate, and the organic phase is dried over sodium sulphate and concentrated under reduced pressure. The residue is subjected to kugelrohr distillation. This gives 15.2 g (79.1% of theory) of 5,6-difluoro-(3-fluorophenoxy)-pyrimidine of boiling point 95° C. at 0.5 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06683029B1 |
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| 出典データセット | uspto-grants-2004_01 |
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| ORD ID | ord-d32f779d34df45009dd0456ed55a88ee |
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| 出典メモ | uspto-grants-2004_01 |
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