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Acetic Acid → 1-(4-Ethynylphenyl)ethan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Ethanone, 1-[4-[(trimethylsilyl)ethynyl]phenyl]- | HCID 11746050 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-(4-Ethynylphenyl)ethan-1-one | HCID 5123626 | 95% |
反応手順
To a stirring solution of compound 1.9 (19 g, 88 mmol) in MeOH (200 mL) was added a solution of KOH (2.46 g, 44 mmol) in MeOH (20 mL) at 10° C. and the mixture was stirred at room temperature for 1 hr. AcOH was added until the pH was 7, and the reaction mixture was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (200 mL), washed with 5% aqueous NaHCO3 (100 mL), brine (100 mL), dried, and concentrated under reduced pressure to give compound 1.10 as a white solid (12 g, 95%). 1H NMR (400 MHz, DMSO-d6) δ 7.95 (d, J=8, 2H), 7.62 (d, J=8, 2H), 4.49 (s, 1H), 2.59 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09403758B2 |
| 出典データセット | uspto-grants-2016_08 |
| ORD ID | ord-472a892854d6416ebc9ff2b2d52c43b7 |
| 出典メモ | uspto-grants-2016_08 |