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Water → 4-Phenylsulfonylphenylethyne
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(Benzenesulfonyl)benzaldehyde | HCID 14417477 | — |
| 反応物 | (1Z)-1-diazo-1-diethoxyphosphorylpropan-2-one | HCID 136104435 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Phenylsulfonylphenylethyne | HCID 19939320 | 42% |
反応手順
To a mixture of 4-(phenylsulfonyl)benzaldehyde (8 g, 32.5 mmol) and potassium carbonate (8.97 g, 65 mmol) in methanol (400 mL) was added diethyl (1-diazo-2-oxopropyl)phosphonate (8.6 g, 39 mmol). The reaction was stirred at room temperature for 3 days then poured into water (600 mL) and extracted with ethyl acetate (×3). The combined organic layers were dried and evaporated. The residue was purified by flash column chromatography on silica, eluting with 5% ethyl acetate/isohexane, to give 1-ethynyl-4-(phenylsulfonyl)benzene (3.3 g, 42%). δH (500 MHz, CDCl3): 7.94-7.88 (4H, m), 7.60-7.50 (5H, m), 3.23 (1H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07468393B2 |
| 出典データセット | uspto-grants-2008_12 |
| ORD ID | ord-bd1663955d9d4cf88849a93a36e9a7cd |
| 出典メモ | uspto-grants-2008_12 |