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publicationDate 2016-04-06-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-105461690-A
titleOfInvention Preparation method of high-purity tert-butyl ((5-(2-fluorophenyl)-1-(pyridine-3-yl sulfonyl)-1H-pyrrole-3-yl)methyl)(methyl)carbamate
abstract 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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