1,3-DIBROMO-2,4-DIFLUOROBENZENE

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1,3-dibromo-2,4-difluoro-benzene (5 g, 18.5 mmol) and pyrrolidin-2-one (1.56 g, 18.5 mmol) in dioxane (160 ml) were stirred under argon. Cs2CO3 (7.19 g, 22 mmol), xantphos (1.27 g, 2 mmol) and Pd2(dba)3 (0.675 g, 0.5 mmol) were added and the reaction was heated to 85° C. for 16 h. The reaction was quenched by the addition of 150 ml of H2O. After extraction with ethyl acetate (three times), the combined organic layers were washed with water, dried with Na2SO4, evaporated to dryness and the product was purified by silica gel chromatography (ethyl acetate/cyclohexane 0 to 20% ethyl acetate). Yield: 1 g, 20 The reaction was quenched by the addition of 150 ml of H2O After extraction with ethyl acetate (three times) the combined organic layers were washed with water dried with Na2SO4 evaporated to dryness the product was purified by silica gel chromatography (ethyl acetate/cyclohexane 0 to 20% ethyl acetate)

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1,3-dibromo-2,4-difluoro-benzene (5 g, 18.5 mmol) and pyrrolidin-2-one (1.56 g, 18.5 mmol) in dioxane (160 ml) were stirred under argon. Cs2CO3 (7.19 g, 22 mmol), xantphos (1.27 g, 2 mmol) and Pd2(dba)3 (0.675 g, 0.5 mmol) were added and the reaction was heated to 85° C. for 16 h. The reaction was quenched by the addition of 150 ml of H2O. After extraction with ethyl acetate (three times), the combined organic layers were washed with water, dried with Na2SO4, evaporated to dryness and the product was purified by silica gel chromatography (ethyl acetate/cyclohexane 0 to 20% ethyl acetate). Yield: 1 g, 20 The reaction was quenched by the addition of 150 ml of H2O After extraction with ethyl acetate (three times) the combined organic layers were washed with water dried with Na2SO4 evaporated to dryness the product was purified by silica gel chromatography (ethyl acetate/cyclohexane 0 to 20% ethyl acetate)

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1,3-dibromo-2,4-difluoro-benzene (5 g, 18.5 mmol) and pyrrolidin-2-one (1.56 g, 18.5 mmol) in dioxane (160 ml) were stirred under argon. Cs2CO3 (7.19 g, 22 mmol), xantphos (1.27 g, 2 mmol) and Pd2(dba)3 (0.675 g, 0.5 mmol) were added and the reaction was heated to 85° C. for 16 h. The reaction was quenched by the addition of 150 ml of H2O. After extraction with ethyl acetate (three times), the combined organic layers were washed with water, dried with Na2SO4, evaporated to dryness and the product was purified by silica gel chromatography (ethyl acetate/cyclohexane 0 to 20% ethyl acetate). Yield: 1 g, 20 The reaction was quenched by the addition of 150 ml of H2O After extraction with ethyl acetate (three times) the combined organic layers were washed with water dried with Na2SO4 evaporated to dryness the product was purified by silica gel chromatography (ethyl acetate/cyclohexane 0 to 20% ethyl acetate)