化学合成。
化学合成
合成路线 1(1. 合成:515131-35-8)
产率:71%
合成条件:With potassium acetate In N,N-dimethyl-formamide at 100℃; for 6 h; Inert atmosphere
实验步骤:参考实施例8 4-甲基-3-(4,4,5,5-四甲基-1,3,2-二氧杂硼杂环戊烷-2-基)苯甲酸(化合物A8)3-碘-4-甲基苯甲酸(26.2g)将100mmol)溶于DMF(300mL)中,然后加入双(pinacolate)二硼(38.1g,150mmol),[1,1'-双(二苯基膦基)二茂铁)二氯化钯(8.17g,10.0mmol)和钾向其中加入乙酸酯(49.0g,500mmol),然后在氩气氛下在100℃下搅拌6小时。向反应混合物中加入1mol / L盐酸,用乙酸乙酯萃取,有机层用盐水洗涤,然后用无水硫酸镁干燥,加入活性炭(1g),接着在室温下搅拌1小时。将反应混合物通过硅藻土过滤,然后用乙酸乙酯洗涤:蒸发溶剂,所得晶体用异丙醚重结晶,然后过滤,得到化合物A8(18.5g,71%)。 1H NMR(300MHz,CDCl3)δ(ppm)1.36(s,12H),2.61(s,3H),7.26(d,J = 8.1Hz,1H),8.02(dd,J = 8.1,1.8Hz,1H ),8.49(d,J = 1.8Hz,1H)。
参考文献:
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