反应详情

温度

140 °C

A mixture of N-{4-[2-chloro-6-(4-trifluoromethyl-phenyl)-pyrimidin-4-yloxy]-benzo[d]thiazol-2-yl}-acetamide (70 mg, 0.15 mmol, Example 7(d)) and 1-ethyl-3-hydroxypiperidine (39 mg, 0.3 mmol, Aldrich) in ethanol (1 mL) was heated in a microwave synthesizer at 140° C. for 20 min. The reaction mixture was diluted with sat. aqueous solution of NaHCO3 (10 mL) and extracted with EtOAc (2×30 mL). The combined organic extracts were washed with brine (20 mL), dried over Na2SO4, and filtered. The filtrate was concentrated in vacuo and the residue was purified by preparative HPLC [gradient 20-80% MeCN (0.1% TFA)/H2O (0.1% TFA)] to give the title compound as a salt with TFA. MS (ESI, pos. ion) m/z: 516 (M+1).

1. extractionextracted with EtOAc (2×30 mL)
2. washThe combined organic extracts were washed with brine (20 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationThe filtrate was concentrated in vacuo
6. customthe residue was purified by preparative HPLC [gradient 20-80% MeCN (0.1% TFA)/H2O (0.1% TFA)]