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HRID 556137作成日:2026年10月26日

Methanol → 1,4-Diethynylbenzene

https://huagongshe.com/reaction/556137

反応式

関与物質

役割名称HCID仕込み量
反応物MethanolHCID 887—
反応物Potassium HydroxideHCID 14797—
反応物1,4-Bis[(trimethylsilyl)ethynyl]benzeneHCID 522492—
溶媒DichloromethaneHCID 6344—
生成物1,4-DiethynylbenzeneHCID 12046363%

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US08053588B2
出典データセットuspto-grants-2011_11
ORD IDord-9574e9ea5d0444d1bfa9af81def54763
出典メモuspto-grants-2011_11