関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 8-(2,6-Difluoro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonitrile | HCID 59292874 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 溶媒 | Diethylether water | HCID 21584184 | — |
| 生成物 | 8-(2,6-Difluoro-3,5-dimethoxy-phenyl)quinoxaline-5-carboxylic acid | HCID 59292834 | — |
反応手順
A solution of KOH (2.4 g, 42.8 mmol, 10 equiv) in H2O (10 mL) was added to 8-(2,6-difluoro-3,5-dimethoxy-phenyl)-quinoxaline-5-carbonitrile (Step 88.2) (1.4 g mg, 4.3 mmol) in ethylene glycol (20 mL). The reaction mixture was stirred at 150° C. for 4 h, allowed to cool to rt, diluted with Et2O/H2O, and extracted with Et2O. The aqueous phase was acidified to pH 5 by addition of 6 N HCl. Vacuum filtration of the resulting suspension afforded 1.47 g of the title compound as a brown solid, which was used without further purification: ESI-MS: 347.1 [M+H]+; tR=4.22 min (System 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536175B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-a5a8986a6b90407f9491745da542121e |
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| 出典メモ | uspto-grants-2013_09 |
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