1-phenylhexane-1,4-dione

反応条件: temp:115.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-phenyl-hexane-1,4-dione (5 g), ethanol amine (1.6 g) and pivalic acid (2.15 g) in a solvent mixture containing n-heptane:tetrahydrofuran:toluene (4:1:1, 50 mL) was refluxed with stirring at 110-120° C. Water formed during the reaction was removed azeotropically during 3 to 4 hrs. The reaction mixture was cooled and the solvent was removed. The residue obtained was dissolved in dichloromethane (50 mL), washed with saturated sodium bicarbonate solution (50 mL), water (50 mL), and then with brine (50 mL), dried (Na2SO4) and the solvent was evaporated. The crude compound obtained as an oily mass. The crude substance was used in the next step without purification. was refluxed was removed azeotropically during 3 to 4 hrs The reaction mixture was cooled the solvent was removed The residue obtained washed with saturated sodium bicarbonate solution (50 mL), water (50 mL) with brine (50 mL), dried (Na2SO4) the solvent was evaporated

反応条件: temp:115.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-phenyl-hexane-1,4-dione (5 g), ethanol amine (1.6 g) and pivalic acid (2.15 g) in a solvent mixture containing n-heptane:tetrahydrofuran:toluene (4:1:1, 50 mL) was refluxed with stirring at 110-120° C. Water formed during the reaction was removed azeotropically during 3 to 4 hrs. The reaction mixture was cooled and the solvent was removed. The residue obtained was dissolved in dichloromethane (50 mL), washed with saturated sodium bicarbonate solution (50 mL), water (50 mL), and then with brine (50 mL), dried (Na2SO4) and the solvent was evaporated. The crude compound obtained as an oily mass. The crude substance was used in the next step without purification. was refluxed was removed azeotropically during 3 to 4 hrs The reaction mixture was cooled the solvent was removed The residue obtained washed with saturated sodium bicarbonate solution (50 mL), water (50 mL) with brine (50 mL), dried (Na2SO4) the solvent was evaporated

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

実験手順: A mixture of 1-phenyl-hexane-1,4-dione (5 g), ethanol amine (1.6 g) and pivalic acid (2.15 g) in a solvent mixture containing n-heptane:tetrahydrofuran:toluene (4:1:1, 50 mL) was refluxed with stirring at 110–120° C. Water formed during the reaction was removed azeotropically during 3 to 4 hrs. The reaction mixture was cooled and the solvent was removed. The residue obtained was dissolved in dichloromethane (50 mL), washed with saturated sodium bicarbonate solution (50 mL), water (50 mL), and then with brine (50 mL), dried (Na2SO4) and the solvent was evaporated. The crude compound obtained as an oily mass. The crude substance was used in the next step without purification. was refluxed was removed azeotropically during 3 to 4 hrs The reaction mixture was cooled the solvent was removed The residue obtained washed with saturated sodium bicarbonate solution (50 mL), water (50 mL) with brine (50 mL), dried (Na2SO4) the solvent was evaporated

反応条件: temp:115.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-phenyl-hexane-1,4-dione (5 g), ethanol amine (1.6 g) and pivalic acid (2.15 g) in a solvent mixture containing n-heptane:tetrahydrofuran:toluene (4:1:1, 50 mL) was refluxed with stirring at 110-120° C. Water formed during the reaction was removed azeotropically during 3 to 4 hrs. The reaction mixture was cooled and the solvent was removed. The residue obtained was dissolved in dichloromethane (50 mL), washed with saturated sodium bicarbonate solution (50 mL), water (50 mL), and then with brine (50 mL), dried (Na2SO4) and the solvent was evaporated. The crude compound obtained as an oily mass. The crude substance was used in the next step without purification. was refluxed was removed azeotropically during 3 to 4 hrs The reaction mixture was cooled the solvent was removed The residue obtained washed with saturated sodium bicarbonate solution (50 mL), water (50 mL) with brine (50 mL), dried (Na2SO4) the solvent was evaporated

反応条件: temp:115.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-phenyl-hexane-1,4-dione (5 g), ethanol amine (1.6 g) and pivalic acid (2.15 g) in a solvent mixture containing n-heptane:tetrahydrofuran:toluene (4:1:1, 50 mL) was refluxed with stirring at 110-120° C. Water formed during the reaction was removed azeotropically during 3 to 4 hrs. The reaction mixture was cooled and the solvent was removed. The residue obtained was dissolved in dichloromethane (50 mL), washed with saturated sodium bicarbonate solution (50 mL), water (50 mL), and then with brine (50 mL), dried (Na2SO4) and the solvent was evaporated. The crude compound obtained as an oily mass. The crude substance was used in the next step without purification. was refluxed was removed azeotropically during 3 to 4 hrs The reaction mixture was cooled the solvent was removed The residue obtained washed with saturated sodium bicarbonate solution (50 mL), water (50 mL) with brine (50 mL), dried (Na2SO4) the solvent was evaporated