化工社化工社 化学情報印刷レポート · 研究参考用
Triphenylphosphine → (3-(4-((1,3-Dioxolan-2-yl)methyl)benzyloxy)phenyl)-(phenyl)methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 3-Hydroxybenzophenone | HCID 83050 | — |
| 反応物 | (4-((1,3-Dioxolan-2-yl)methyl)phenyl)methanol | HCID 86676898 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (3-(4-((1,3-Dioxolan-2-yl)methyl)benzyloxy)phenyl)-(phenyl)methanone | HCID 71113108 | 117.8% |
反応手順
To a cooled (0° C.) solution of (4-((1,3-dioxolan-2-yl)methyl)phenyl)methanol (0.45 g, 2.317 mmol), 3-hydroxybenzophenone (0.551 g, 2.78 mmol) and triphenylphosphine (0.729 g, 2.78 mmol) in anhydrous THF, di-iso-propylazodicarboxylate (1.027 mL, 2.78 mmol) was added dropwise. The reaction mixture was allowed to warm to RT and stirred at this temperature for 16 hours. The reaction mixture was diluted with ethyl acetate and washed with 10% aqueous potassium carbonate, brine and dried (magnesium sulfate). The suspension was filtered and concentrated under reduced pressure. The crude material was purified by silica gel chromatography eluting with 100% iso-hexane to 25% ethyl acetate in iso-hexane to afford the title compound (1.022 g, >100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08877774B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-25d0f516749b4f2e97a0a4f49ecfd867 |
| 出典メモ | uspto-grants-2014_11 |