221615-72-1Relevant articles and documents
Selective Late-Stage Oxygenation of Sulfides with Ground-State Oxygen by Uranyl Photocatalysis
Li, Yiming,Rizvi, S. Aal-e-Ali,Hu, Deqing,Sun, Danwen,Gao, Anhui,Zhou, Yubo,Li, Jia,Jiang, Xuefeng
supporting information, p. 13499 - 13506 (2019/08/21)
Oxygenation is a fundamental transformation in synthesis. Herein, we describe the selective late-stage oxygenation of sulfur-containing complex molecules with ground-state oxygen under ambient conditions. The high oxidation potential of the active uranyl cation (UO22+) enabled the efficient synthesis of sulfones. The ligand-to-metal charge transfer process (LMCT) from O 2p to U 5f within the O=U=O group, which generates a UV center and an oxygen radical, is assumed to be affected by the solvent and additives, and can be tuned to promote selective sulfoxidation. This tunable strategy enabled the batch synthesis of 32 pharmaceuticals and analogues by late-stage oxygenation in an atom- and step-efficient manner.
Preparation of relying on tests the past intermediate 1 - (6 - methyl pyridine - 3 - yl) - 2 - [4 - (methylsulfonyl) phenyl] ethanone method
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Paragraph 0045-0046, (2017/08/25)
The invention provides a preparation method of 1-(6-methylpyridyl-3-yl)-2-[4-(mesyl)-phenyl]-ethyl-one, which is characterized by comprising the following steps: (1) adding a compound B and an organic metal reagent into (4-dimethylsulfido)phenylacetic acid or metal salt (A) thereof to perform condensation reaction to obtain a compound C disclosed in the specification, wherein M is selected from H or metals and is preferably H or an alkali metal, and R is selected from H or C1-C6 alkyl groups; and (2) oxidizing the compound C with oxydol to obtain a compound D disclosed in the specification. In the two-step synthesis process, the yield from the compound A to the compound C is about 85%, the yield from the compound C to the compound D is about 90%, and the total mole yield is 65-80%; and the HPLC (high performance liquid chromatography) purity of the compound D is higher than 98%.Compared with the prior art, the method provided by the invention has the advantages of higher product quality and lower cost.
PROCESS FOR CYCLOOXYGENASE-2 SELECTIVE INHIBITOR
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Paragraph 0099, (2013/09/26)
The present invention describes a process for preparing a cyclooxygenase-2 selective inhibitor. It provides a synthetic procedure for the said substance namely 5-chloro-3-(4-methylsulphonyl)phenyl-2-(2-methyl-5-pyridinyl)pyridine of formula (I). The invention also relates to preparation of a new intermediate of formula (IV) and a process to prepare it. Furthermore, the invention describes a process for preparing another key intermediate of formula (II). Compounds of formula (IV) and formula (II) are useful intermediates in synthesis of the said cyclooxygenase-2 inhibitor.
