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向NaH(12.9g,0.322mol,60%分散于礦物油中)的無(wú)水THF(500mL)懸浮液中緩慢滴加乙二醇(20.0g,0.322mol)的無(wú)水THF(100mL)溶液。室溫下攪拌反應(yīng)混合物1小時(shí)后,加入叔丁基二甲基氯硅烷(TBSCl,48.59g,0.322mol),繼續(xù)在室溫下攪拌1小時(shí)。反應(yīng)完成后,用10%的K2CO3水溶液(100mL)淬滅反應(yīng),隨后用甲基叔丁基醚(MTBE,3×300mL)萃取。合并有機(jī)相,用無(wú)水Na2SO4干燥,過(guò)濾后減壓濃縮。粗產(chǎn)物通過(guò)硅膠柱色譜法純化,采用1%至33%乙酸乙酯的石油醚溶液進(jìn)行梯度洗脫,得到2-((叔丁基二甲基甲硅烷基)氧基)乙醇(55.0g,收率96%),為無(wú)色油狀物。
參考文獻(xiàn):
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[2] Organic Letters, 2016, vol. 18, # 18, p. 4534 - 4537
[3] Patent: US2016/122318, 2016, A1. Location in patent: Paragraph 0181
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