関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 反応物 | 3-bromo-N-[2-hydroxy-5-(trifluoromethyl)phenyl]isonicotinamide | HCID 66879880 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(3-Bromopyridin-4-yl)-5-(trifluoromethyl)benzoxazole | HCID 66880917 | 87.1% |
反応手順
To a mixture of 0.29 g of 3-bromo-N-[2-hydroxy-5-(trifluoromethyl)phenyl]isonicotinamide, 4 ml of tetrahydrofuran and 0.25 g of triphenylphosphine, 0.42 g of 40% toluene solution of diethyl azodicarboxylate was added dropwise at room temperature. The reaction mixture was stirred while heating at 50° C. for 1.5 hours. The reaction mixture was cooled to room temperature, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 0.24 g of 2-(3-bromopyridin-4-yl)-5-(trifluoromethyl)benzoxazole (hereinafter, referred to as “active compound 27”).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08609705B2 |
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| 出典データセット | uspto-grants-2013_12 |
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| ORD ID | ord-5086dda980724981977988f9deade821 |
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| 出典メモ | uspto-grants-2013_12 |
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