化学合成。
化学合成
合成路线 1(1. 合成:4687-25-6)
产率:74%
合成条件:With selenium(IV) oxide In 1,4-dioxane for 24 h; Reflux
实验步骤:将3-甲基苯并呋喃(200mg,0.19ml,1.5mmol)和SeO 2(200mg,1.8mmol,1.2当量)悬浮在1,4-二恶烷(3ml)中并加热回流24小时。 使反应混合物冷却,然后用EtOAc /己烷(2:1v / v,10ml)稀释,并通过短的二氧化硅塞过滤以除去硒残余物。 将二氧化硅塞用EtOAc(2×3ml)洗涤,将合并的有机滤液蒸发至干,通过硅胶柱色谱法(己烷/ EtOAc 96:4)纯化,得到黄色油状物(162mg,1.1mmol,74%)。 百分比产量)。 1 H NMR(300MHz,CDCl 3)δ10.18(s,1H),8.26(s,1H),8.19(m,1H),7.54(m,1H),7.41(m,2H); ESI m / z = 147.0(MH)+,计算值。 对于C9H702 = 147.04。
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