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Raw materials And Preparation Products

Questions And Answer

• Preparation

  Sodium thiophenolate is prepared by the following steps:A solution of (11) ( 1.0 g, 2.8 mmol), phenylthiol (0.33 g, 3.0 mmol), acetonitrile  (5 cm3) and sodium carbonate (0.3 g) was stirred under reflux for 19 h. Water (20 cm3)  was added, then the mixture extracted into DCM. The DCM solution was dried (MgS04)  and evaporated to dryness. Chromatography on silica gel with DCM - hexane (30 : 70) as  the eluent yielded 2,6-dibromo-3,5-difluoro-4-thiophenoxypyridine (0.9 g, 85%), m.p.65.5-66.5 OC (Found: C, 34.45; H, 1.3; N, 3.2. C11H5Bf2F2NS requires C, 34.7; H,  1.3; N, 3.7%); IR spectrum no. 16; mass spectrum no. 19; nmr spectrum no. 16.;

Spectrum Detail