12-aminododecan-1-ol

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: In 600 ml of methanol was dissolved while warming 48.0 g of N-(12-hydroxydodecyl)phthalimide, 50 ml of hydrazine monohydrate was added at room temperature with stirring and the mixture was stirred overnight. The crystal thus separated out was filtered off and the solvent was distilled off. The residue was extracted with hot chloroform and insolubles were filtered off. The filtrate was distilled, the residue was extracted with hot chloroform (100 ml×3) and then the solvent was distilled off. The residue was dissolved in methanol and recrystallization from methanol-ethyl acetate gave 21.6 g of the title compound as a crystal. was added at room temperature the mixture was stirred overnight The crystal thus separated out was filtered off the solvent was distilled off The residue was extracted with hot chloroform and insolubles were filtered off The filtrate was distilled the residue was extracted with hot chloroform (100 ml×3) the solvent was distilled off The residue was dissolved in methanol recrystallization from methanol-ethyl acetate

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

実験手順: An aqueous solution of 100 mg of 12-aminododecanol in 57% hydriodic acid was heated under reflux for one hour. To the reaction solution was added chloroform and the mixture was washed successively with water, a 10% aqueous solution of sodium thiosulfate and a saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue thus obtained was chromatographed over a silica gel column to afford 171 mg of the title compound. under reflux for one hour the mixture was washed successively with water a 10% aqueous solution of sodium thiosulfate and a saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate The solvent was distilled off the residue thus obtained was chromatographed over a silica gel column

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

実験手順: An aqueous solution of 100 mg of 12-aminododecanol in 57% hydriodic acid was heated under reflux for one hour. To the reaction solution was added chloroform and the mixture was washed successively with water, a 10% aqueous solution of sodium thiosulfate and a saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue thus obtained was chromatographed over a silica gel column to afford 171 mg of the title compound. under reflux for one hour the mixture was washed successively with water a 10% aqueous solution of sodium thiosulfate and a saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate The solvent was distilled off the residue thus obtained was chromatographed over a silica gel column

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

実験手順: To 4.07 g of potassium 6-(4-ethyl-1-piperazinyl)-pyridine-3-carboxylate and 3.00 g of 12-aminododecanol was added 50 ml of methylene chloride and then 2.86 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (WSCI) and 2.01 g of 1-hydroxybenzotriazole (HOBt) were added while stirring at room temperature. The mixture was stirred at room temperature for 15 hours. To the reaction solution were added water and diisopropyl ether and subsequent filtration and drying under reduced pressure afforded 5.67 g of the title compound as a crystal. The mixture was stirred at room temperature for 15 hours To the reaction solution were added water and diisopropyl ether and subsequent filtration drying under reduced pressure

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

実験手順: To 4.07 g of potassium 6-(4-ethyl-1-piperazinyl)-pyridine-3-carboxylate and 3.00 g of 12-aminododecanol was added 50 ml of chloroform and then 2.01 g of 1-hydroxybenzotriazole (HOBt) and 3.07 g of 1,3-dicyclohexylcarbodiimide (DCC) were added thereto while stirring at room temperature and then the mixture was stirred at room temperature for 17 hours. A further 50 ml of chloroform was added, the mixture was stirred and then insolubles were filtered off. After the residue on a filter paper was washed with chloroform, the washing and the chloroform solution were combined and washed with a 10% aqueous solution of sodium hydroxide and dried over anhydrous magnesium sulfate. After the chloroform solution was concentrated, diisopropyl ether was added and the crystal thus separated out was recovered by filtration and dried under reduced pressure to afford 5.10 g of the title compound as a crystal. the mixture was stirred at room temperature for 17 hours the mixture was stirred insolubles were filtered off After the residue on a filter paper was washed with chloroform washed with a 10% aqueous solution of sodium hydroxide dried over anhydrous magnesium sulfate After the chloroform solution was concentrated diisopropyl ether was added the crystal thus separated out was recovered by filtration dried under reduced pressure

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

実験手順: To 4.07 g of potassium 6-(4-ethyl-1-piperazinyl)-pyridine-3-carboxylate and 3.00 g of 12-aminododecanol was added 50 ml of chloroform and then 2.01 g of 1-hydroxybenzotriazole (HOBt) and 3.07 g of 1,3-dicyclohexylcarbodiimide (DCC) were added thereto while stirring at room temperature and then the mixture was stirred at room temperature for 17 hours. A further 50 ml of chloroform was added, the mixture was stirred and then insolubles were filtered off. After the residue on a filter paper was washed with chloroform, the washing and the chloroform solution were combined and washed with a 10% aqueous solution of sodium hydroxide and dried over anhydrous magnesium sulfate. After the chloroform solution was concentrated, diisopropyl ether was added and the crystal thus separated out was recovered by filtration and dried under reduced pressure to afford 5.10 g of the title compound as a crystal. the mixture was stirred at room temperature for 17 hours the mixture was stirred insolubles were filtered off After the residue on a filter paper was washed with chloroform washed with a 10% aqueous solution of sodium hydroxide dried over anhydrous magnesium sulfate After the chloroform solution was concentrated diisopropyl ether was added the crystal thus separated out was recovered by filtration dried under reduced pressure

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: An ethanol solution (100 ml) of 12-aminododecanol (4.81 g, 23.9 mmol) and trifluoroacetic acid ethyl ester (6.79 g, 47.8 mmol) was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure to give 12-trifluoroacetamidododecanol (1) (6.98 g, q.) as a colorless syrup. The reaction mixture was concentrated under reduced pressure

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

実験手順: In 600 ml of methanol was dissolved while warming 48.0 g of N-(12-hydroxydodecyl)phthalimide, 50 ml of hydrazine monohydrate was added at room temperature with stirring and the mixture was stirred overnight. The crystal thus separated out was filtered off and the solvent was distilled off. The residue was extracted with hot chloroform and insolubles were filtered off. The filtrate was distilled, the residue was extracted with hot chloroform (100 ml×3) and then the solvent was distilled off. The residue was dissolved in methanol and recrystallization from methanol-ethyl acetate gave 21.6 g of the title compound as a crystal. was added at room temperature the mixture was stirred overnight The crystal thus separated out was filtered off the solvent was distilled off The residue was extracted with hot chloroform and insolubles were filtered off The filtrate was distilled the residue was extracted with hot chloroform (100 ml×3) the solvent was distilled off The residue was dissolved in methanol recrystallization from methanol-ethyl acetate

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

実験手順: An aqueous solution of 100 mg of 12-aminododecanol in 57% hydriodic acid was heated under reflux for one hour. To the reaction solution was added chloroform and the mixture was washed successively with water, a 10% aqueous solution of sodium thiosulfate and a saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue thus obtained was chromatographed over a silica gel column to afford 171 mg of the title compound. under reflux for one hour the mixture was washed successively with water a 10% aqueous solution of sodium thiosulfate and a saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate The solvent was distilled off the residue thus obtained was chromatographed over a silica gel column

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

実験手順: To 4.07 g of potassium 6-(4-ethyl-1-piperazinyl)-pyridine-3-carboxylate and 3.00 g of 12-aminododecanol was added 50 ml of methylene chloride and then 2.86 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (WSCI) and 2.01 g of 1-hydroxybenzotriazole (HOBt) were added while stirring at room temperature. The mixture was stirred at room temperature for 15 hours. To the reaction solution were added water and diisopropyl ether and subsequent filtration and drying under reduced pressure afforded 5.67 g of the title compound as a crystal. The mixture was stirred at room temperature for 15 hours To the reaction solution were added water and diisopropyl ether and subsequent filtration drying under reduced pressure