反应详情

Sodium hydride (0.104 g, 2.6 mmol, 60% suspension in mineral oil, Aldrich) was added in small portions to a solution of benzo[b]thiophen-4-ol (0.3 g, 2 mmol, prepared according WO 01/68653) in DMF (4 mL) and the mixture was stirred at room temperature for 0.5 h. (4-Chloro-6-(4-trifluoromethyl-phenyl)-pyrimidine, (Example 2(a), Method A), (0.776 g, 3 mmol) was then added and the mixture was stirred at room temperature for 18 h. The solvent was evaporated under vacuum, the residue was dissolved in EtOAc (50 mL), washed with 1 N NaOH and water, dried over MgSO4, and filtered. The filtrate was evaporated under vacuum and the residue purified by silica gel chromatography (10% EtOAc in hexanes) to give the title compound. Mp: 122.3-122.4° C. MS (ESI, pos. ion) m/z: 373.1 (M+1).

1. additionwas then added
2. customThe solvent was evaporated under vacuum
3. dissolutionthe residue was dissolved in EtOAc (50 mL)
4. washwashed with 1 N NaOH and water
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customThe filtrate was evaporated under vacuum
8. customthe residue purified by silica gel chromatography (10% EtOAc in hexanes)