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With caesium carbonate; In N,N-dimethyl-formamide; at 29 - 70℃; for 2h;
To a mixture of compound 168(2.00g. 10.3 Immol) and 16 (1.72g. 12.37mmol) in DMF (2OmL), was added C52CO3(672g, 20.62mmoi) in one portion at 29CThe mixture was heated to 70C and stirred for 2 hours. LCMS showed the reaction was completed. The mixture was cooled to29C and concentrated in reduced pressure at 40C. The residue was poured into water (4OmL) and stilTed for 5 minutes. The aqueous phase was extracted with EtOAc(8OrnLx2). The combined organic phase was washed with saturated brine (2OmL), dried with anhydrous Na2SO4, filtered and concentrated in vacuum. The residue was purified by silica gel chromatography to afford product 169 (150g. yield: 4647%). ?H NMR (400 MHz, CDCI3): c37.62- 7.84 (m, 3H), 7.28-7.26 (m, I H), 6.68-6.67 (m, I H).
With caesium carbonate; In N,N-dimethyl-formamide; at 80℃; for 1.5h;Inert atmosphere;
To a mixture of 180 (193.97mg, i.OOrnrnol) and 28 (139.10mg, i.OOrnmol) in DMF (5rnL), was added C52CO3 (325.82mg, 1 .OOmmol) in one portion at room temperature. The mixture was then heated to 80uC for 1 5 hours under N2 atmosphere. ILC showed the reaction was completed. Themixture was cooled to room temperature and was then poured into water (i5mL) slowly. A white solid precipitated out from the mixture, filtered off. The solid was dried to afford product 197 (300.00 mg, yield: 67.08%).LCMS: m/, 313.9 (M±H.
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