反应详情

温度

125 °C

A mixture of N-{4-[2-chloro-6-(4-trifluoromethyl-phenyl)-pyrimidin-4-yloxy]-benzothiazol-2-yl}-acetamide (186 mg, 0.4 mmol, Example 7(d)) and tert-butyl 1-piperazine-carboxylate (149 mg, 0.8 mmol, Aldrich) in ethanol (1 mL) was heated in a microwave synthesizer at 125° C. for 40 min. The reaction mixture was evaporated under reduced pressure and the residue was treated with sat. aqueous solution of NaHCO3 (10 mL), and extracted with EtOAc (2×30 mL). The combined EtOAc extracts were washed with brine, dried over Na2SO4 and filtered. The filtrate was evaporated in vacuo and the residue was purified by silica gel column chromatography (20% EtOAc/hexane) to give the title compound as a solid. MS (ESI, pos. ion) m/z: 615 (M+1). M.p.: 211° C.

1. customThe reaction mixture was evaporated under reduced pressure
2. additionthe residue was treated with sat. aqueous solution of NaHCO3 (10 mL)
3. extractionextracted with EtOAc (2×30 mL)
4. washThe combined EtOAc extracts were washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customThe filtrate was evaporated in vacuo
8. customthe residue was purified by silica gel column chromatography (20% EtOAc/hexane)