[H-].C[O:3]CCO[Al+]OCCOC.[Na+].[H-].[Br:15][C:16]1[CH:21]=[CH:20][C:19]([S:22][CH:23]2[CH2:25][CH2:24]2)=[C:18]([Cl:26])[CH:17]=1.CO.[OH2:29]>O1CCCC1>[Br:15][C:16]1[CH:21]=[CH:20][C:19]([S:22]([CH:23]2[CH2:24][CH2:25]2)(=[O:3])=[O:29])=[C:18]([Cl:26])[CH:17]=1
Oxone(R) (20.3 g) was added to a solution of 4-bromo-2-chloro-1-(cyclopropylsulfanyl)benzene obtained in Reference Example 5-22 (964 mg) in tetrahydrofuran (20 mL)-methanol (20 mL)-water (10 mL), and the mixture was stirred at room temperature for one day. Oxone(R) (6.8 g) was further added and the mixture was stirred at room temperature for 18 hours. Water was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform only) to give the title compound as a pale yellow amorphous (597 mg, 55%).
Wird geladen…
