反应详情

温度

120 °C

A mixture of N-{4-[2-chloro-6-(4-trifluoromethyl-phenyl)-pyrimidin-4-yloxy]-benzo[d]thiazol-2-yl}-acetamide (465 mg, 1.0 mmol, Example 7(d)), 4-fluoro-α-methylbenzyl-alcohol (140 mg, 1 mmol, Aldrich), K2CO3 (207 mg, 1.5 mmol) and 85% MeSO2Na (30 mg, 0.25 mmol, Aldrich) in DMF (50 mL) was heated at 120° C. with stirring for 5 h. The reaction mixture was allowed to reach room temperature and was diluted with water (50 mL), and exacted with EtOAc (2×50 mL). The organic phase was washed with brine (10 mL), dried over Na2SO4, and filtered. The filtrate was evaporated in vacuo and the residue purified by silica gel column chromatography (20% EtOAc/hexane) to give the title compound. MS (ESI, pos. ion) m/z: 569 (M+1).

1. customto reach room temperature
2. washThe organic phase was washed with brine (10 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customThe filtrate was evaporated in vacuo
6. customthe residue purified by silica gel column chromatography (20% EtOAc/hexane)