関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Chlorodifluoromethane | HCID 6372 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-[5-(Trifluoromethyl)benzoxazole-2-yl]pyridin-3-ol | HCID 136331268 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(3-Difluoromethoxypyridin-4-yl)-5-(trifluoromethyl)benzoxazole | HCID 66880475 | — |
反応手順
A mixture of 0.50 g of 4-[5-(trifluoromethyl)benzoxazole-2-yl]pyridin-3-ol, 1.23 g of potassium carbonate and 14 ml of DMF was stirred while heating at 70° C. for three hours with chlorodifluoromethane gas injected. By stopping injection of gas, the mixture was cooled to room temperature and allowed to stand overnight. Water was added to the reaction mixture, followed by extraction with ethyl acetate twice. The combined organic layers were washed with water and a saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 0.11 g of 2-(3-difluoromethoxypyridin-4-yl)-5-(trifluoromethyl)benzoxazole (hereinafter, referred to as “active compound 126”).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08445522B2 |
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| 出典データセット | uspto-grants-2013_05 |
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| ORD ID | ord-01f8da89aa7c4173ba32f2ef38f20842 |
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| 出典メモ | uspto-grants-2013_05 |
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