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Methanol → 1,4-Diethynylbenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1,4-Bis[(trimethylsilyl)ethynyl]benzene | HCID 522492 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,4-Diethynylbenzene | HCID 120463 | 63% |
反応手順
Subsequently, the obtained 1,4-bis(trimethylsilylethynyl)benzene (500 mg, 1.85 mmol) was added with dist. CH2Cl2 (15 mL), dist. MeOH (3 mL) and an aqueous solution of potassium hydroxide (KOH) (0.4 mL) of 50% by mass. The resultant mixture was stirred under a nitrogen atmosphere at room temperature for 18 hours to obtain a reaction mixture. Then, the reaction mixture was diluted with CH2Cl2. After that, an organic layer was washed with sat. NaCl, and dried with MgSO4. The dried organic layer was filtered and concentrated to obtain a crude product. Subsequently, the obtained crude product was separated and purified by silica gel column chromatography (hexane/EtOAc=20/1) to obtain 1,4-diethynylbenzene (147 mg, 63% yield (in two steps)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08053588B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-9574e9ea5d0444d1bfa9af81def54763 |
| 出典メモ | uspto-grants-2011_11 |