反应详情

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)).

1. customto obtain a reaction mixture
2. washAfter that, an organic layer was washed with sat. NaCl
3. dry with materialdried with MgSO4
4. filtrationThe dried organic layer was filtered
5. concentrationconcentrated
6. customto obtain a crude product
7. customSubsequently, the obtained crude product
8. customwas separated
9. custompurified by silica gel column chromatography (hexane/EtOAc=20/1)