関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Dimethylhydroxymethyl-4-acetylphenylacetylene | HCID 66784133 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(4-Ethynylphenyl)ethan-1-one | HCID 5123626 | 56% |
反応手順
1.45 g (7.17 mmol) of dimethylhydroxymethyl-4-acetylphenylacetylene and 301 mg (7.53 mmol) of NaOH (KISHIDA CHEMICAL CO., Ltd., 0.7 mm granular, 98%) were placed in a 100 mL two-neck flask equipped with a reflux condenser and the air inside the flask was replaced with Ar. 36 mL of toluene was added thereto and the mixture was refluxed at 120° C. for 15 minutes. Toluene was added to the reaction mixture and the mixture was washed with a saturated aqueous ammonium chloride solution and dried over magnesium sulfate, followed by distilling off of the solvent under reduced pressure by an evaporator. Then, 25 mL of hexane was added to the resulting crude reaction product and the mixture was cooled to give 4-acetylphenylethyne as a yellow solid. (0.74 g, yield: 56%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08137821B2 |
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| 出典データセット | uspto-grants-2012_03 |
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| ORD ID | ord-51a39bf682344d698bde5af78593cdee |
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| 出典メモ | uspto-grants-2012_03 |
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