3-methyl-1-phenylbutan-2-one

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A solution of benzaldehyde (6.5g, 0.0617 mole), 3-methyl-1-phenyl-2-butanone (10 g, 0.0617 mole) and piperidine (0.2 g) in benzene (50 ml) was heated to reflux for 20 hours. Water formed during the reaction was removed (azeotrope) by the use of a Dean-Stark trap. The reaction was concentrated to an oil, and the product was purified by silica gel chromatography. to reflux for 20 hours was removed (azeotrope) by the use of a Dean-Stark trap The reaction was concentrated to an oil the product was purified by silica gel chromatography

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

実験手順: 31 g (0.25 mol) of 4-fluorobenzaldehyde, 40.6 g (0.25 mol) of benzyl isopropyl ketone, 2.5 ml of piperidine and 1.75 ml of glacial acetic acid are boiled in a water separator for 20 hours in 200 ml of toluene. After removing the solvent, the residue is distilled through a 20 cm Vigreux column. After removing the solvent the residue is distilled through a 20 cm Vigreux column

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

実験手順: 31 g (0.25 mol) of 4-fluorobenzaldehyde, 40.6 g (0.25 mol) of benzyl isopropyl ketone, 2.5 ml of piperidine and 1.75 ml of glacial acetic acid are boiled in a water separator for 20 hours in 200 ml of toluene. After removing the solvent, the residue is distilled through a 20 cm Vigreux column. After removing the solvent the residue is distilled through a 20 cm Vigreux column

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

実験手順: 0.9 ml of piperidine is added to 24.8 g (0.2 mol) of 4-fluorobenzaldehyde and 32.4 g (0.2 mol) of benzyl isopropyl ketone in 150 ml of toluene and the mixture is heated to reflux overnight. After cooling to room temperature, the mixture is extracted several times using water and the organic phase is dried over magnesium sulphate and concentrated in vacuo. The residue is subjected to incipient distillation up to a bath temperature of 150° C. at 0.1 mbar in a high vacuum and 43.8 g of crude product are obtained in the distillation residue. the mixture is heated to reflux overnight the mixture is extracted several times the organic phase is dried over magnesium sulphate concentrated in vacuo distillation up to a bath temperature of 150° C. at 0.1 mbar in a high vacuum and 43.8 g of crude product are obtained in the distillation residue

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

実験手順: A solution of benzaldehyde (6.5g, 0.0617 mole), 3-methyl-1-phenyl-2-butanone (10 g, 0.0617 mole) and piperidine (0.2 g) in benzene (50 ml) was heated to reflux for 20 hours. Water formed during the reaction was removed (azeotrope) by the use of a Dean-Stark trap. The reaction was concentrated to an oil, and the product was purified by silica gel chromatography. to reflux for 20 hours was removed (azeotrope) by the use of a Dean-Stark trap The reaction was concentrated to an oil the product was purified by silica gel chromatography

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

実験手順: A solution of benzaldehyde (6.5g, 0.0617 mole), 3-methyl-1-phenyl-2-butanone (10 g, 0.0617 mole) and piperidine (0.2 g) in benzene (50 ml) was heated to reflux for 20 hours. Water formed during the reaction was removed (azeotrope) by the use of a Dean-Stark trap. The reaction was concentrated to an oil, and the product was purified by silica gel chromatography. to reflux for 20 hours was removed (azeotrope) by the use of a Dean-Stark trap The reaction was concentrated to an oil the product was purified by silica gel chromatography

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: The procedure described in Example 1 was repeated by using 2.96 g of 2-methyl-4-phenyl-3-butanone and 2.4 g of 3,4-dihydroxy-5-nitrobenzaldehyde. Yield 0.52 g, mp 151°-156° C.

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

実験手順: 0.9 ml of piperidine is added to 24.8 g (0.2 mol) of 4-fluorobenzaldehyde and 32.4 g (0.2 mol) of benzyl isopropyl ketone in 150 ml of toluene and the mixture is heated to reflux overnight. After cooling to room temperature, the mixture is extracted several times using water and the organic phase is dried over magnesium sulphate and concentrated in vacuo. The residue is subjected to incipient distillation up to a bath temperature of 150° C. at 0.1 mbar in a high vacuum and 43.8 g of crude product are obtained in the distillation residue. the mixture is heated to reflux overnight the mixture is extracted several times the organic phase is dried over magnesium sulphate concentrated in vacuo distillation up to a bath temperature of 150° C. at 0.1 mbar in a high vacuum and 43.8 g of crude product are obtained in the distillation residue

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

実験手順: 0.9 ml of piperidine is added to 24.8 g (0.2 mol) of 4-fluorobenzaldehyde and 32.4 g (0.2 mol) of benzyl isopropyl ketone in 150 ml of toluene and the mixture is heated to reflux overnight. After cooling to room temperature, the mixture is extracted several times using water and the organic phase is dried over magnesium sulphate and concentrated in vacuo. The residue is subjected to incipient distillation up to a bath temperature of 150° C. at 0.1 mbar in a high vacuum and 43.8 g of crude product are obtained in the distillation residue. the mixture is heated to reflux overnight the mixture is extracted several times the organic phase is dried over magnesium sulphate concentrated in vacuo distillation up to a bath temperature of 150° C. at 0.1 mbar in a high vacuum and 43.8 g of crude product are obtained in the distillation residue

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

実験手順: 31 g (0.25 mol) of 4-fluorobenzaldehyde, 40.6 g (0.25 mol) of benzyl isopropyl ketone, 2.5 ml of piperidine and 1.75 ml of glacial acetic acid are boiled in a water separator for 20 hours in 200 ml of toluene. After removing the solvent, the residue is distilled through a 20 cm Vigreux column. After removing the solvent the residue is distilled through a 20 cm Vigreux column