反应详情

温度

20 °C

A solution of cyclopropane-1,1-diyldimethanol (3.7 g) dissolved in ethylene glycol dimethyl ether (50 mL) was treated with 60% sodium hydride (1.449 g) at 0° C. under nitrogen. The resulting mixture was stirred at 20° C. for 1 h, treated with tert-butylchlorodimethylsilane (5.46 g) and stirred at room temperature overnight. The reaction mixture was diluted with water (250 mL), and extracted with ethyl acetate (2×250 mL). The organic was dried (MgSO4), filtered and evaporated to afford crude product. The crude product was purified (SiO2 chromatography, elution 100% DCM). Pure fractions were evaporated to dryness to afford the subtitle compound (5.50 g) as an oil.

1. stirringstirred at room temperature overnight
2. extractionextracted with ethyl acetate (2×250 mL)
3. dry with materialThe organic was dried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customto afford crude product
7. customThe crude product was purified
8. wash(SiO2 chromatography, elution 100% DCM)
9. customPure fractions were evaporated to dryness