化学合成。
化学合成
合成路线 1(1. 合成:32936-76-8)
产率:62%
合成条件:Stage #1: With n-butyllithium; diisopropylamine In tetrahydrofuran; hexane at 0℃; for 0.50 h; Stage #2: at 20℃; for 3 h;
实验步骤:实施例B19将0℃的二异丙胺(17mL,121mmol)的THF(50mL)溶液用正丁基锂(2.5M的己烷溶液,48mL,120mmol)处理,搅拌10分钟,用 环丁烷羧酸(5.00g,49.9mmol)并搅拌0.5小时。 加入甲基碘(9.00g,63.4mmol),将混合物在室温下搅拌3小时,然后浓缩至干。 将混合物用饱和NaHCO 3处理。 用DCM(2x)萃取NH 4 Cl,并将合并的有机物用盐水洗涤,用Na 2 SO 4干燥并浓缩至干,得到1-甲基环丁烷羧酸(3.54g,62%),为棕色油状物。
参考文献:
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