化学合成。
化学合成
合成路线 1(1. 合成:784-77-0)
产率:96%
合成条件:at 0℃; for 2 h;
实验步骤:步骤1:3-硝基-4-(三氟甲氧基)苯甲酸(270)的合成得到4-(三氟甲氧基)苯甲酸(900mg,4.37mmol)的浓盐酸溶液。 将H 2 SO 4(9ml)在0℃冷却,得到硝酸钾(486mg,4.80mmol)的浓溶液。 加入H 2 SO 4(4.5ml),并将反应在相同温度下搅拌2小时。 将混合物用H 2 O(50ml)处理,并用EtOAc(150ml)萃取。 将有机相用盐水(2×100ml)洗涤,用Na 2 SO 4干燥并蒸发至干,得到3-硝基-4-(三氟甲氧基)苯甲酸(2)(1.05g,4.18mmol,96%收率,MS / ESI + 252.1)。[MH] +)。 该产物无需纯化即可使用。
参考文献:
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