1-decylpiperazine

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:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 53.4 Grams of 1-ethoxycarbonyl-4-decylpiperazine is combined with 300 ml. of concentrated hydrochloric acid and refluxed with stirring under a nitrogen atmosphere for approximately 48 hours. After cooling to room terperature the solvents are removed under reduced pressure. The resulting solid is suspended in ethanol, filtered, and air-dried to yield 1-decylpiperazine. After cooling to room terperature the solvents are removed under reduced pressure filtered air-dried

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

実験手順: 53.4 Grams of 1-ethoxycarbonyl-4-decylpiperazine is combined with 300 ml. of concentrated hydrochloric acid and refluxed with stirring under a nitrogen atmosphere for approximately 48 hours. After cooling to room terperature the solvents are removed under reduced pressure. The resulting solid is suspended in ethanol, filtered, and air-dried to yield 1-decylpiperazine. After cooling to room terperature the solvents are removed under reduced pressure filtered air-dried

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2.02 g of ethyl 1-piperazinecarboxylate, 1.92 g of anhydrous potassium carbonate, 3.08 g of decyl bromide and 20 ml of 2-butanone was stirred overnight at 80° C. After addition of water, the reaction mixture was extracted with ethyl acetate. The ethyl acetate layer was extracted with 3N hydrochloric acid. The extract was made alkaline with potassium carbonate and then extracted with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure Ethanol (20 ml) and ml of 10% aqueous sodium hydroxide were added to the residue, and the mixture was stirred overnight at 100° C. The reaction mixture was cooled and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 0.38 g of 1-decylpiperazine as an oil. the reaction mixture was extracted with ethyl acetate The ethyl acetate layer was extracted with 3N hydrochloric acid extracted with ethyl acetate The extract was washed with water dried over anhydrous sodium sulfate concentrated under reduced pressure Ethanol (20 ml) and ml of 10% aqueous sodium hydroxide were added to the residue the mixture was stirred overnight at 100° C The reaction mixture was cooled extracted with ethyl acetate The extract was washed with water dried over anhydrous sodium sulfate concentrated under reduced pressure

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

実験手順: 53.4 Grams of 1-ethoxycarbonyl-4-decylpiperazine is combined with 300 ml. of concentrated hydrochloric acid and refluxed with stirring under a nitrogen atmosphere for approximately 48 hours. After cooling to room terperature the solvents are removed under reduced pressure. The resulting solid is suspended in ethanol, filtered, and air-dried to yield 1-decylpiperazine. After cooling to room terperature the solvents are removed under reduced pressure filtered air-dried

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

実験手順: A 2.3 g (8.64 mmoles) quantity of N,N,-dicyclohexylcarbodiimide was added to 20 ml of a solution of 2.0 g (7.35 mmoles) of N-decylpiperazine, 1.9 g (7.56 mmoles) of N-t-butoxycarbonylphenylglycine, 1.3 g (15.5 mmoles) of sodium hydrogen carbonate and 122 mg (1.0 mmole) of 4-dimethylaminopyridine in anhydrous methylene chloride. The mixture was stirred at room temperature for 12 hours. The precipitated crystals were collected by filtration and washed with methylene chloride. Mother liquor and the washings were concentrated under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=15:1), giving 2.8 g (yield: 83%) of 1-(N-t-butoxycarbonylphenylglycyl)-4-decylpiperazine. The precipitated crystals were collected by filtration washed with methylene chloride Mother liquor and the washings were concentrated under reduced pressure the residue was purified by silica gel column chromatography (chloroform:methanol=15:1)

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

実験手順: The title compound of Example 2 (1.0 g, 3.4 mmol) was combined with 1-decylpiperazine (0.77 g, 3.4 mmol) and the reaction was carried out by the method of Example 4. Following chromatographic purification, 1.08 g of the title product was obtained. purification

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 20 g (0.18 mole) quantity of N-formylpiperazine, 37.2 ml (0.18 mole) of 1-bromodecane and 25 g (0.18 mole) of potassium carbonate were suspended in 20 ml of N,N-dimethylformamide and the suspension was stirred at 80° C. for 3 hours. The suspension was further extracted with 300 ml of benzene, and the organic layer was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was dissolved in 80 ml of methanol, and 20 ml of concentrated hydrochloric acid was added thereto and the mixture was refluxed for 3 hours. The solvent was evaporated under reduced pressure and the precipitated crystals were washed with acetone, giving 35.6 g (yield: 66%) of N-decylpiperazine as the hydrochloride. The suspension was further extracted with 300 ml of benzene the organic layer was washed with water dried over anhydrous magnesium sulfate concentrated under reduced pressure The residue was dissolved in 80 ml of methanol 20 ml of concentrated hydrochloric acid was added the mixture was refluxed for 3 hours The solvent was evaporated under reduced pressure the precipitated crystals were washed with acetone

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2.02 g of ethyl 1-piperazinecarboxylate, 1.92 g of anhydrous potassium carbonate, 3.08 g of decyl bromide and 20 ml of 2-butanone was stirred overnight at 80° C. After addition of water, the reaction mixture was extracted with ethyl acetate. The ethyl acetate layer was extracted with 3N hydrochloric acid. The extract was made alkaline with potassium carbonate and then extracted with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure Ethanol (20 ml) and ml of 10% aqueous sodium hydroxide were added to the residue, and the mixture was stirred overnight at 100° C. The reaction mixture was cooled and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 0.38 g of 1-decylpiperazine as an oil. the reaction mixture was extracted with ethyl acetate The ethyl acetate layer was extracted with 3N hydrochloric acid extracted with ethyl acetate The extract was washed with water dried over anhydrous sodium sulfate concentrated under reduced pressure Ethanol (20 ml) and ml of 10% aqueous sodium hydroxide were added to the residue the mixture was stirred overnight at 100° C The reaction mixture was cooled extracted with ethyl acetate The extract was washed with water dried over anhydrous sodium sulfate concentrated under reduced pressure

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

実験手順: 53.4 Grams of 1-ethoxycarbonyl-4-decylpiperazine is combined with 300 ml. of concentrated hydrochloric acid and refluxed with stirring under a nitrogen atmosphere for approximately 48 hours. After cooling to room terperature the solvents are removed under reduced pressure. The resulting solid is suspended in ethanol, filtered, and air-dried to yield 1-decylpiperazine. After cooling to room terperature the solvents are removed under reduced pressure filtered air-dried