反应详情

温度

80 °C

Firstly, dist. toluene (5 mL) was added to and dissolved in 1-(diallylethoxysilyl)-4-(3,5-dimethyl-3-hydroxy-hexynyl)benzene (125 mg, 0.35 mmol) obtained in Synthesis example 10. The resultant mixture was added with NaOH (9.9 mg, 0.25 mmol), and then was stirred under a nitrogen atmosphere at 80° C. for 16 hours to obtain a reaction mixture. Then, the reaction mixture was diluted with CH2Cl2, and an organic layer was washed with dist. H2O and sat. NaCl. The organic layer thus collected was dried with MgSO4, and 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=5/1) to obtain 1-(diallylethoxysilyl)-4-ethynylbenzene (5 mg, 6% yield).

1. customobtained in Synthesis example 10
2. customto obtain a reaction mixture
3. washan organic layer was washed with dist
4. customThe organic layer thus collected
5. dry with materialwas dried with MgSO4
6. filtrationthe dried organic layer was filtered
7. concentrationconcentrated
8. customto obtain a crude product
9. customThe obtained crude product
10. customwas separated
11. custompurified by silica gel column chromatography (hexane/EtOAc=5/1)