作为医药中间体或活性成分,用于相关药物研发(如专利US2011/144097等文献报道)。
医药
合成路线 1(1. 合成:1310350-99-2)
产率:95%
合成条件:Stage #1: With water; lithium hydroxide In tetrahydrofuran; methanol at 20℃; for 1 h; Stage #2: With hydrogenchloride In water
实验步骤:c)4-氯-1-二氟甲基-1H-吡唑-3-羧酸4-氯-1-二氟甲基-1H-吡唑-3-甲酸甲酯(540mg,2.6mmol)的四氢呋喃溶液(18ml) 在室温下用氢氧化锂(135mg,5.6mmol)在1:1的水和甲醇(12ml)混合物中的溶液处理.1小时后反应完成,溶剂在蒸发时减少。 将残余物溶于水(10ml)中,用盐酸(2M)酸化。用乙酸乙酯萃取,用硫酸钠干燥有机层,减压蒸发,得到白色固体(555mg),为白色固体。 用戊烷(10ml)研磨。过滤固体物质,用戊烷洗涤并干燥。减压干燥后,得到4-氯-1-二氟甲基-1H-吡唑-3-羧酸,为白色固体(477)。 mg,理论值的95%)。 MS(ISP):m / z = 195.0 [M-H] - 。
参考文献:
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