反应详情

温度

110 °C

2-{2-[1-(5-chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethanamine from step 3 of this example (50 mg, 0.178 mmol) was in 0.594 mL NMP. 1-fluoro-4-(methylsulfonyl)benzene (37.2 mg, 0.2141 mol) and DBU (0.040 mL, 0.267 mmol) were sequentially added. The reaction mixture was stirred at 110° C. overnight before cooled back to room temperature. The reaction mixture was diluted with water and aqueous phase was further extracted with ethyl acetate for 3 times. The combined organic layers were washed with water and brine, then dried over Na2SO4 and concentrated. The residue was purified by column chromatography using gradient elution (0 to 65% ethyl acetate in hexane) to give the titled compound. LRMS calc: 434.9; obs: 435 (M+1).

1. temperaturebefore cooled back to room temperature
2. extractionwas further extracted with ethyl acetate for 3 times
3. washThe combined organic layers were washed with water and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residue was purified by column chromatography
7. washelution (0 to 65% ethyl acetate in hexane)