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5-(2-fluoro-4-methyl-5-nitrophenyl)-1-methylpyridin-2(1H)-one[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
99%
With bis-triphenylphosphine-palladium(II) chloride; sodium carbonate; In 1,2-dimethoxyethane; water; at 120℃; for 0.5h;Inert atmosphere; Microwave irradiation;
4-bromo-5- fluoro-2-nitrotoluene (Aldrich, 0.234 g, 1.0 mmol), l-methyl-5-(4,4,5,5-tetramethyl-[1,3,2]dioxaboralan-2-yl)-1H-pyridin-2-one (Synchem, Inc.0.235 g, 1.0 mmol), bis(triphenylphosphine)palladium(II) chloride (0.035 g, 0.05 mmol) and sodium carbonate 2M (1.5 mL, 3.0 mmol) were combined in DME (4 mL) and water (4.0 mL), sparged with nitrogen and heated by microwave at 120 °C for 30 minutes. The reaction mixture was partitioned between ethyl acetate and water. The ethyl acetate layer was washed with brine, dried (Na2SO4), treated with mercaptopropyl silica gel for 30 minutes, filtered and concentrated to afford the title compound (0.262 g, 99percent).
99%
With bis-triphenylphosphine-palladium(II) chloride; sodium carbonate; In 1,2-dimethoxyethane; water; at 120℃; for 0.5h;Inert atmosphere; Microwave irradiation;
Example 257A 5-(2-fluoro-4-methyl-5-nitrophenyl)-1-methylpyridin-2(1H)-one [1076] 4-bromo-5-fluoro-2-nitrotoluene (Aldrich, 0.234 g, 1.0 mmol), 1-methyl-5-(4,4,5,5-tetramethyl-[1,3,2]dioxaboralan-2-yl)-1H-pyridin-2-one (Synchem, Inc. 0.235 g, 1.0 mmol), bis(triphenylphosphine)palladium(II)chloride (0.035 g, 0.05 mmol) and sodium carbonate 2M (1.5 mL, 3.0 mmol) were combined in DME (4 mL) and water (4.0 mL), sparged with nitrogen and heated by microwave at 120° C. for 30 minutes. The reaction mixture was partitioned between ethyl acetate and water. The ethyl acetate layer was washed with brine, dried (Na2SO4), treated with mercaptopropyl silica gel for 30 minutes, filtered and concentrated to afford the title compound (0.262 g, 99percent).
Chemistry
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120K+ Compounds
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