反应详情

温度

0 °C

2,2′-(1,3-Phenylene)diethanol (0.430 g, 2.59 mmol) and imidazole (0.176 g, 2.59 mmol) were dissolved in anhydrous N,N-dimethylformamide (15 mL) and cooled to 0° C. in an ice bath. Chlorotriisopropylsilane (0.22 mL) was slowly added and the reaction mixture was kept stirring at 0° C. for 3 h, and then diluted with water (5 mL), extracted with ethyl acetate (15 mL×2), and washed with brine (10 mL×2). The organic layer was dried over anhydrous sodium sulfate, filtered, and evaporated to dryness. The residue so obtained was purified by column chromatography eluting with 1:10 of ethyl acetate-hexanes to give the desired compound as a colorless oil. Yield 35%.

1. extractionextracted with ethyl acetate (15 mL×2)
2. washwashed with brine (10 mL×2)
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. filtrationfiltered
5. customevaporated to dryness
6. customThe residue so obtained
7. customwas purified by column chromatography
8. washeluting with 1:10 of ethyl acetate-hexanes