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发明授权
CN105461690B 高纯度((5-(2-氟苯基)-1-(吡啶-3-基磺酰基)-1H-吡咯-3-基)甲基)(甲基)氨基甲酸叔丁酯的制备方法 有权

高纯度((5-(2-氟苯基)-1-(吡啶-3-基磺酰基)-1H-吡咯-3-基)甲基)(甲基)氨基甲酸叔丁酯的制备方法
摘要：
本发明公开了高纯度((5‑(2‑氟苯基)‑1‑(吡啶‑3‑基磺酰基)‑1H‑吡咯‑3‑基)甲基)(甲基)氨基甲酸叔丁酯的制备方法，包括以下步骤：将((5‑(2‑氟苯基)‑1H‑吡咯‑3‑基)‑N‑甲基)甲基氨基甲酸叔丁酯溶解于有机溶剂，加入氢化钠，升温反应后在低温条件下滴加3‑吡啶磺酰氯，搅拌反应1‑3h，过滤得到((5‑(2‑氟苯基)‑1‑(吡啶‑3‑基磺酰基)‑1H‑吡咯‑3‑基)甲基)(甲基)氨基甲酸叔丁酯粗品溶液；将该溶液加入纯化水，调节pH至弱酸性，降温搅拌析晶抽滤，滤饼干燥后用异丙醚、正庚烷混合溶液打浆，抽滤、干燥得到高纯度产品。本发明工艺简单，安全可靠，制备的富马酸沃诺拉赞中间体((5‑(2‑氟苯基)‑1‑(吡啶‑3‑基磺酰基)‑1H‑吡咯‑3‑基)甲基)(甲基)氨基甲酸叔丁酯的产率和纯度高，适合工业化放大生产。
摘要（英）：

The invention discloses a preparation method of high-purity tert-butyl ((5-(2-fluorophenyl)-1-(pyridine-3-yl sulfonyl)-1H-pyrrole-3-yl)methyl)(methyl)carbamate, which comprises the following steps: dissolving tert-butyl ((5-(2-fluorophenyl)-1H-pyrrole-3-yl)-N-methyl)methyl carbamate in an organic solvent, adding sodium hydride, heating for reacting, dropwise adding 3-pyridine sulfonyl chloride at low temperature, reacting under stirring for 1-3h, and filtering to obtain a solution of a tert-butyl ((5-(2-fluorophenyl)-1-(pyridine-3-yl sulfonyl)-1H-pyrrole-3-yl)methyl)(methyl)carbamate crude product; adding purified water to the solution, adjusting the pH to weak acidity, cooling, stirring, separating out crystals, carrying out suction filtration, drying a filter cake, pulping with an isopropyl ether and n-heptane mixed solution, carrying out suction filtration and drying to obtain a high-purity product. The process is simple, safe and reliable; the prepared vonoprazan fumarate intermediate tert-butyl ((5-(2-fluorophenyl)-1-(pyridine-3-yl sulfonyl)-1H-pyrrole-3-yl)methyl)(methyl)carbamate has high yield and purity, and is suitable for industrialized scaled production.

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