반응 #45803

반응 방정식

trimethylboroxine

5-Amino-2-bromo-6-fluoro-4-methoxy-2-methylbiphenyl-3-carbonitrile

potassium carbonate

1,4-dioxane

→

5-Amino-6-fluoro-4-methoxy-2-methylbiphenyl-3-carbonitrile

용매

water

반응 조건

후처리

1. 1
   온도cooling to room temperature
2. 2
   workup.STIRRINGby further stirring at 110° C. for 11 hours
3. 3
   온도After cooling to room temperature
4. 4
   기타the insoluble matter was separated by filtration
5. 5
   기타The organic layer was separated
6. 6
   추출the aqueous layer was again extracted with ethyl acetate

실험 절차

5-Amino-2-bromo-6-fluoro-4-methoxy-2-methylbiphenyl-3-carbonitrile (I-235) (2.02 g, 6.29 mmol), potassium carbonate (2.61 g, 18.87 mmol) and tetrakis(triphenylphosphine)palladium(0) (727 mg, 0.63 mmol) were dissolved in 10% water-containing 1,4-dioxane (50 ml), and at room temperature, trimethylboroxine (50 wt. % tetrahydrofuran solution, 1.90 ml, 7.55 mmol) was added. After stirring under nitrogen atmosphere at 110° C. for 8 hours and then cooling to room temperature, tetrakis(triphenylphosphine)palladium(0) (727 mg, 0.63 mmol) was added, followed by further stirring at 110° C. for 11 hours. After cooling to room temperature, the insoluble matter was separated by filtration, the filtrate was fractionated with ethyl acetate and saturated brine. The organic layer was separated, the aqueous layer was again extracted with ethyl acetate.

출처