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Triphenylphosphine → 4-(3,4-Dichlorobenzyloxy)-2-methoxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 3,4-Dichlorobenzyl alcohol | HCID 15728 | — |
| 反応物 | 4-Hydroxy-2-Methoxybenzaldehyde | HCID 519541 | — |
| 反応物 | Diethylazodicarboxylate toluene | HCID 66777355 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(3,4-Dichlorobenzyloxy)-2-methoxybenzaldehyde | HCID 77231379 | 96.1% |
反応手順
4-Hydroxy-2-methoxybenzaldehyde (408 mg, 2.68 mmol), 3,4-dichlorobenzyl alcohol (665 mg, 3.76 mmol), and triphenylphosphine (980 mg, 3.74 mmol) were dissolved in tetrahydrofuran (8 mL), and a diethyl azodicarboxylate toluene solution (2.2 M, 1.71 mL, 3.76 mmol) was slowly added dropwise thereto at room temperature, and then, the resulting mixture was stirred under a nitrogen atmosphere at room temperature for 2 hours. The solvent in the reaction solution was distilled off under reduced pressure, and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 90:10 (v/v)), whereby the objective title compound was obtained as a white solid (801 mg, yield: 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08222281B2 |
| 出典データセット | uspto-grants-2012_07 |
| ORD ID | ord-6db5d53681db4b2db030822ec8022df2 |
| 出典メモ | uspto-grants-2012_07 |