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Triphenylphosphine → 2-[5-Chloro-2-(3-methylisoxazol-5-ylmethoxy)benzyl]isoindole-1,3-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 反応物 | (3-Methylisoxazol-5-yl)methanol | HCID 10820493 | — |
| 反応物 | 2-[5-Chloro-2-hydroxy benzyl]isoindole-1,3-dione | HCID 21973298 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-[5-Chloro-2-(3-methylisoxazol-5-ylmethoxy)benzyl]isoindole-1,3-dione | HCID 22661767 | 52.2% |
反応手順
To a mixture of 2-[5-chloro-2-hydroxy benzyl]isoindole-1,3-dione (800 mg, 2.78 mmol), 5-hydroxymethyl-3-methyl-isoxazole (373 mg, 3.3 mmol), and triphenylphosphine (1.0 g, 4.2 mmol) in anhydrous THF (10 mL) was added diethylazodicarboxylate (0.657 mL, 4.7 mmol). The solution was stirred for 15 h at room temperature under anhydrous conditions. The solvent was then removed by rotary evaporation and the product was preadsorbed onto silica gel and purified by flash chromatography to afford the title compound (555 mg, 52%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06803457B1 |
| 出典データセット | uspto-grants-2004_10 |
| ORD ID | ord-3127d714a8fd4ac9837dc84b1d6b7271 |
| 出典メモ | uspto-grants-2004_10 |