化学合成。
化学合成
合成路线 1(1. 合成:138786-86-4)
产率:100%
合成条件:Stage #1: at 20℃; for 16 h; Stage #2: With water; sodium hydrogencarbonate In methanol; ethyl acetate
实验步骤:参考例1 4-硝基-1H-吡唑-3-羧酸甲酯将乙酰氯(9mL)滴加到甲醇(90mL),4-硝基-1H-吡唑-3-羧酸(9.00g,57.3mmol)中 加入混合物中。 将混合物在室温下搅拌16小时,并减压浓缩。 向残余物中加入甲醇,并将混合物减压浓缩,重复该操作两次。 将残余物用甲醇和乙酸乙酯稀释。 加入5%碳酸氢钠水溶液,将pH调节至8-9。 用乙酸乙酯萃取混合物。 萃取液用水,盐水洗涤,用无水硫酸镁干燥,减压蒸发溶剂,得到标题化合物(9.83g,收率100%)。 1H-NMR(DMSO-d6,200MHz):δ3.98(3H,s),8.28(1H,s)。
参考文献:
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