1-(2-benzoylethyl)piperidinium chloride

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

実験手順: In 470 ml of water were dissolved 60.2 g of β-piperidinopropiophenone hydrochloride and 18.1 g of hydroxylamine hydrochloride. To this solution was added portionwise 21.9 g of sodium hydrogencarbonate. After the whole amount was added, the mixture was stirred overnight. To the stirred mixture was then added an aqueous solution of 14.2 g of sodium hydroxide in 47 ml of water. Thus obtained mixture was well stirred and allowed to stand for 2 hours to produce a white precipitate. The precipitate was collected by filtration and washed successively with two portions of 200 ml of water and ethanol. The washed precipitate was dried to obtain a white solid. The solid was then recrystallized from methanol to obtain 41.2 g (yield: 74.8%) of the subject compound as a silver-white scaly product. After the whole amount was added Thus obtained mixture was well stirred to stand for 2 hours to produce a white precipitate The precipitate was collected by filtration washed successively with two portions of 200 ml of water and ethanol The washed precipitate was dried to obtain a white solid The solid was then recrystallized from methanol

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

実験手順: A mixture of 120 g of acetophenone, 133 g of piperidine hydrochloride and 50 g of paraformaldehyde in 120 ml of ethanol was refluxed for 6 hours. The mixture was then allowed to stand for cooling to soldify. The resulting solid was crushed after addition of 400 ml of acetone, and then collected by filtration. The collected solid was washed successively with acetone and hexane and dried to obtain 191.6 g (yield: 75.4%) of the subject compound as a white scaly product. was refluxed for 6 hours for cooling The resulting solid was crushed collected by filtration The collected solid was washed successively with acetone and hexane dried

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

実験手順: In 470 ml of water were dissolved 60.2 g of β-piperidinopropiophenone hydrochloride and 18.1 g of hydroxylamine hydrochloride. To this solution was added portionwise 21.9 g of sodium hydrogencarbonate. After the whole amount was added, the mixture was stirred overnight. To the stirred mixture was then added an aqueous solution of 14.2 g of sodium hydroxide in 47 ml of water. Thus obtained mixture was well stirred and allowed to stand for 2 hours to produce a white precipitate. The precipitate was collected by filtration and washed successively with two portions of 200 ml of water and ethanol. The washed precipitate was dried to obtain a white solid. The solid was then recrystallized from methanol to obtain 41.2 g (yield: 74.8%) of the subject compound as a silver-white scaly product. After the whole amount was added Thus obtained mixture was well stirred to stand for 2 hours to produce a white precipitate The precipitate was collected by filtration washed successively with two portions of 200 ml of water and ethanol The washed precipitate was dried to obtain a white solid The solid was then recrystallized from methanol

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

実験手順: A mixture of 120 g of acetophenone, 133 g of piperidine hydrochloride and 50 g of paraformaldehyde in 120 ml of ethanol was refluxed for 6 hours. The mixture was then allowed to stand for cooling to soldify. The resulting solid was crushed after addition of 400 ml of acetone, and then collected by filtration. The collected solid was washed successively with acetone and hexane and dried to obtain 191.6 g (yield: 75.4%) of the subject compound as a white scaly product. was refluxed for 6 hours for cooling The resulting solid was crushed collected by filtration The collected solid was washed successively with acetone and hexane dried

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

実験手順: In 470 ml of water were dissolved 60.2 g of β-piperidinopropiophenone hydrochloride and 18.1 g of hydroxylamine hydrochloride. To this solution was added portionwise 21.9 g of sodium hydrogencarbonate. After the whole amount was added, the mixture was stirred overnight. To the stirred mixture was then added an aqueous solution of 14.2 g of sodium hydroxide in 47 ml of water. Thus obtained mixture was well stirred and allowed to stand for 2 hours to produce a white precipitate. The precipitate was collected by filtration and washed successively with two portions of 200 ml of water and ethanol. The washed precipitate was dried to obtain a white solid. The solid was then recrystallized from methanol to obtain 41.2 g (yield: 74.8%) of the subject compound as a silver-white scaly product. After the whole amount was added Thus obtained mixture was well stirred to stand for 2 hours to produce a white precipitate The precipitate was collected by filtration washed successively with two portions of 200 ml of water and ethanol The washed precipitate was dried to obtain a white solid The solid was then recrystallized from methanol

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

実験手順: A mixture of 120 g of acetophenone, 133 g of piperidine hydrochloride and 50 g of paraformaldehyde in 120 ml of ethanol was refluxed for 6 hours. The mixture was then allowed to stand for cooling to soldify. The resulting solid was crushed after addition of 400 ml of acetone, and then collected by filtration. The collected solid was washed successively with acetone and hexane and dried to obtain 191.6 g (yield: 75.4%) of the subject compound as a white scaly product. was refluxed for 6 hours for cooling The resulting solid was crushed collected by filtration The collected solid was washed successively with acetone and hexane dried