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:

反応条件: temp:167.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of formic acid (250 ml) and formamide (500 ml) was added 1-phenyl-2-butanone (25 g, 0.168 mols); the reaction was then heated to 165-170° C. for four hours. The reaction was then cooled and poured into water (1 l). The aqueous phase was then extracted with ethyl acetate (3×100 ml). The organic phase was washed with saturated sodium bicarbonate (2×200 ml) and dried over magnesium sulfate. Evaporation of the solvent yielded an oil (24.1 g, 80%). The reaction was then cooled The aqueous phase was then extracted with ethyl acetate (3×100 ml) The organic phase was washed with saturated sodium bicarbonate (2×200 ml) dried over magnesium sulfate Evaporation of the solvent

反応条件: temp:167.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of formic acid (250 ml) and formamide (500 ml) was added 1-phenyl-2-butanone (25 g, 0.168 mols); the reaction was then heated to 165-170° C. for four hours. The reaction was then cooled and poured into water (1 l). The aqueous phase was then extracted with ethyl acetate (3×300 ml). The organic phase was washed with saturated sodium bicarbonate (2×200 ml) and dried over magnesium sulfate. Evaporation of the solvent yielded an oil (24.1 g, 80%). The reaction was then cooled The aqueous phase was then extracted with ethyl acetate (3×300 ml) The organic phase was washed with saturated sodium bicarbonate (2×200 ml) dried over magnesium sulfate Evaporation of the solvent

反応条件: temp:167.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of formic acid (250 ml) and formamide (500 ml) was added 1-phenyl-2-butanone (25 g, 0.168 mols); the reaction was then heated to 165-170° C. for four hours. The reaction was then cooled and poured into water (1 l). The aqueous phase was then extracted with ethyl acetate (3×100 ml). The organic phase was washed with saturated sodium bicarbonate (2×200 ml) and dried over magnesium sulfate. Evaporation of the solvent yielded an oil (24.1 g, 80%). The reaction was then cooled The aqueous phase was then extracted with ethyl acetate (3×100 ml) The organic phase was washed with saturated sodium bicarbonate (2×200 ml) dried over magnesium sulfate Evaporation of the solvent

反応条件: temp:167.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of formic acid (250 ml) and formamide (500 ml) was added 1-phenyl-2-butanone (25 g, 0.168 mols); the reaction was then heated to 165-170° C. for four hours. The reaction was then cooled and poured into water (1 l). The aqueous phase was then extracted with ethyl acetate (3×100 ml). The organic phase was washed with saturated sodium bicarbonate (2×200 ml) and dried over magnesium sulfate. Evaporation of the solvent yielded an oil (24.1 g, 80%). The reaction was then cooled The aqueous phase was then extracted with ethyl acetate (3×100 ml) The organic phase was washed with saturated sodium bicarbonate (2×200 ml) dried over magnesium sulfate Evaporation of the solvent

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

実験手順: Ethyl benzyl ketone is reacted with 1-bromo-3-butene according to the foregoing details and there is obtained 5-phenyl-oct-1-en-6-one of boiling point 106° C./4 mmHg; nD20 =1.5088.

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

実験手順: Ethyl benzyl ketone is reacted with crotyl chloride according to the foregoing details and there is obtained 5-phenyl-oct-2-en-6-one of boiling point 95° C./3 mmHg; nD20 =1.5102.

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

実験手順: If ethyl benzyl ketone is reacted with β-methallyl chloride according to the foregoing details, then there is obtained 2-methyl-4-phenyl-hept-1-en-5-one of boiling point 93° C./3 mmHg; nD20 =1.5094.

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 192 g (2.4 mol) of 50% sodium hydroxide and 6 g of hexadecyl-trimethylammonium bromide are placed in a 2-liter flask provided with a thermometer, stirrer and reflux condenser and there is then added dropwise while stirring within 0.5 hour a mixture of 296 g (2 mol) of ethyl benzyl ketone and 251 g (2.4 mol) of prenyl chloride. The mixture is warmed to 60° C. and stirred for 3 hours. The mixture is left to cool and 500 ml of ice/water are added thereto. The mixture is extracted four times with ether and washed neutral with water. The phase separation can be facilitated by the addition of a small amount of alcohol. After drying over sodium sulphate, the ether is evaporated and a fractional distillation is then carried out. There are thus obtained 224 g of 2-methyl-5-phenyl-oct-2-en-6-one of boiling point 106° C./3 mmHg; nD20 =1.5092-88; yield 75%. provided with a thermometer, stirrer reflux condenser there is then added dropwise stirred for 3 hours The mixture is left to cool The mixture is extracted four times with ether washed neutral with water The phase separation can be facilitated by the addition of a small amount of alcohol After drying over sodium sulphate the ether is evaporated a fractional distillation

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

実験手順: In a 2-liter flask provided with a thermometer, stirrer, dropping funnel and reflux condenser 600 ml of absolute alcohol are treated portionwise while stirring with 30 g of sodium metal and the mixture is held at reflux temperature until the metal has dissolved. Within 0.5 hour there is added dropwise to the boiling solution a mixture of 117.2 g of benzyl cyanide and 153.2 g of ethyl propionate and the mixture is heated for a further 3 hours. The alcohol is then distilled off and there are added 300 ml of toluene, followed by 250 ml of ice/water. The aqueous phase is separated, washed with 300 ml of toluene and then 540 g of 96% sulphuric acid are added. The mixture is held at reflux temperature until the evolution of carbon dioxide ceases, cooled, diluted with 250 ml of ice/water and extracted with two 300 ml portions of toluene. The toluene extracts are washed with water, with 10% sodium carbonate solution and again with water, dried over sodium sulphate and evaporated. Distillation gives 79 g of ethyl benzyl ketone of boiling point 69° C./3 mmHg; nD20 =1.5109; yield 53%. In a 2-liter flask provided with a thermometer, stirrer are treated portionwise at reflux temperature until the metal has dissolved Within 0.5 hour there is added dropwise to the boiling solution the mixture is heated for a further 3 hours The alcohol is then distilled off there are added 300 ml of toluene The aqueous phase is separated washed with 300 ml of toluene 540 g of 96% sulphuric acid are added at reflux temperature until the evolution of carbon dioxide ceases cooled diluted with 250 ml of ice/water extracted with two 300 ml portions of toluene The toluene extracts are washed with water, with 10% sodium carbonate solution and again with water dried over sodium sulphate evaporated Distillation

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

実験手順: Ethyl benzyl ketone is reacted with 1-bromo-3-butene according to the foregoing details and there is obtained 5-phenyl-oct-1-en-6-one of boiling point 106° C./4 mmHg; nD20 =1.5088.