関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene, 1-fluoro-2-methyl-4-nitro- | HCID 68001 | — |
| 反応物 | 3-Bromo-2-hydroxypyridine | HCID 818549 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Bromo-1-(2-methyl-4-nitrophenyl)pyridin-2(1H)-one | HCID 59410157 | — |
反応手順
44.5 g (280 mmol) of 3-bromopyridin-2(1H)-one are dissolved in 750 ml of anhydrous dimethyl sulfoxide and admixed at room temperature with 33.4 g (298 mmol) of potassium tert-butoxide in portions. The suspension is stirred at this temperature for 1 h, before 38.5 g (280 mmol) of 1-fluoro-2-methyl-4-nitrobenzene are added and the reaction solution is heated to 80° C. for 20 h. It is allowed to cool and diluted cautiously with water. The precipitated crystalline solid is filtered off, washed with a little water and dried under reduced pressure. This affords 62 g (80% of theory) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08198267B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-095551dc86b244eb93822301a94506b3 |
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| 出典メモ | uspto-grants-2012_06 |
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