関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 反応物 | 5-Methyloxazolo[4,5-b]pyridin-2(3H)-one | HCID 10012075 | — |
| 反応物 | [3-(5-Methylpyrimidin-2-yl)phenyl]methanol | HCID 59484945 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-methyl-3-[3-(5-methylpyrimidin-2-yl)benzyl]-3H-benzoxazol-2-one | HCID 25125095 | — |
反応手順
112 mg (0.75 mmol) of 5-methyl-3H-oxazolo[4,5-b]pyridin-2-one, 180 mg (0.90 mmol) of [3-(5-methylpyrimidin-2-yl)phenyl]methanol and 238 mg (0.90 mmol) of triphenylphosphine are suspended in 5 ml of THF, and the mixture is stirred for 30 min. The mixture is subsequently cooled to 0° C., and 186 μl (0.90 mmol) of diisopropyl azodicarboxylate are added. The reaction mixture is stirred at room temperature for 2 h. The reaction mixture is diluted with 20 ml of dichloromethane, washed with 2×20 ml of water, dried over sodium sulfate and evaporated. The residue is purified by column chromatography on silica gel; yield: 101 mg of “A45”; ESI: 332 (M+H); Rt=4.91 min (method C);
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08071593B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-4e4fbdd9c9a34a518667459884621da4 |
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| 出典メモ | uspto-grants-2011_12 |
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