反应详情

Firstly, a mixture of 1,4-diiodobenzene (4 g, 12.1 mmol), PdCl2(PPh3)2 (340 mg, 0.484 mmol) and CuI (92.4 mg, 0.484 mmol), was added with dist. THF (20 mL), dist. Et3N (60 mL) and trimethylsilylacetylene (3.77 mL, 26.7 mmol). The resultant mixture was stirred under a nitrogen atmosphere at 80° C. for 22 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. The obtained crude product was separated and purified by silica gel column chromatography (hexane/EtOAc=10/1) to obtain 1,4-diethynylbenzene.

1. additionwas added with dist
2. customto obtain a reaction mixture
3. washAfter that, an organic layer was washed with sat. NaCl
4. dry with materialdried with MgSO4
5. filtrationThe dried organic layer was filtered
6. concentrationconcentrated
7. customto obtain a crude product
8. customThe obtained crude product
9. customwas separated
10. custompurified by silica gel column chromatography (hexane/EtOAc=10/1)