1-hexylpiperazine

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 100 mL of ethanol add 87 g (0.1 mol) of epichlorohydrin and zinc chloride (1 mL of a 0.872M solution in ether). Stir the reaction mixture at 100° C. for 2 days at which time remove the heat source and add 17.0 g (0.1 mol) of 1-hexyl-piperazine and 20 mL of 50% aqueous sodium hydroxide. Heat the reaction for 3 hours. Add 100 mL of water and extract twice with 200 mL of ether. Combine the organic layers and dry over Na2SO4. Remove the drying agent by filtration and evaporate the solvent in vacuo to obtain the title compound. remove the heat source Heat the reaction for 3 hours extract twice with 200 mL of ether dry over Na2SO4 Remove the drying agent by filtration evaporate the solvent in vacuo

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 100 mL of ethanol add 87 g (0.1 mol) of epichlorohydrin and zinc chloride (1 mL of a 0.872M solution in ether). Stir the reaction mixture at 100° C. for 2 days at which time remove the heat source and add 17.0 g (0.1 mol) of 1-hexyl-piperazine and 20 mL of 50% aqueous sodium hydroxide. Heat the reaction for 3 hours. Add 100 mL of water and extract twice with 200 mL of ether. Combine the organic layers and dry over Na2SO4. Remove the drying agent by filtration and evaporate the solvent in vacuo to obtain the title compound. remove the heat source Heat the reaction for 3 hours extract twice with 200 mL of ether dry over Na2SO4 Remove the drying agent by filtration evaporate the solvent in vacuo

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

実験手順: A mixture of 8.5 g (0.05 mole) of a n-hexyl piperazine and 6.8 g (0.056 mole) of 1-chloro-3-pentanone was heated to 140° for 5 minutes. The reaction product was dissolved in isopropanol and acidified with a solution of HCl in isopropanol. The dihydrochloride salt was filtered and crystallized from acetonitrile to give 11.0 g of white solid with a melting point of 230°-233° C. was heated to 140° for 5 minutes The dihydrochloride salt was filtered crystallized from acetonitrile

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 15.3 g (0.09 mole) of n-hexyl piperazine and 12.3 g (0.091 mole) of 1-chloro-3-hexanone was heated to 100° C. for 5 minutes, cooled and dissolved in isopropanol. Isopropanolic HCl was added until acidic. Ether was added and the salt was filtered off. The product was crystallized from acetonitrile to yield 16.5 g of product with a melting point of 225°-230° C. cooled the salt was filtered off The product was crystallized from acetonitrile

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1.8 g (0.01 mole) of n-hexyl piperazine and 1.9 g (0.014 mole) of 1-chloro-3-hexanone was heated to 120° C. for 5 minutes. The reaction product was slurried with ether, filtered and crystallized from acetonitrile to yield 4.2 g of product having a melting point of 162°-164° C. filtered crystallized from acetonitrile

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

実験手順: A solution of 8.5 g (0.07 mole) of 1-chloro-2-hexanone in 25 ml of ether was added dropwise to a mixture of 8.5 g (0.05 mole) of a n-hexyl piperazine and 10 g (0.1 mole) of triethylamine in 50 ml of ether. Addition was completed in 1 hour and the reaction mixture was stirred for 48 hours. The reaction mixture was filtered and the solvent was removed. The residue was dissolved in water, basified with 50% NaOH and extracted into toluene. The toluene was evaporated and the residue was treated with a saturated solution of HCl in isopropanol. The salt was filtered and crystallized twice from isopropanol to yield 6.2 g with a melting point of 190°-192° C. Addition The reaction mixture was filtered the solvent was removed The residue was dissolved in water extracted into toluene The toluene was evaporated the residue was treated with a saturated solution of HCl in isopropanol The salt was filtered crystallized twice from isopropanol to yield 6.2 g with a melting point of 190°-192° C.

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 100 mL of ethanol add 87 g (0.1 mol) of epichlorohydrin and zinc chloride (1 mL of a 0.872M solution in ether). Stir the reaction mixture at 100° C. for 2 days at which time remove the heat source and add 17.0 g (0.1 mol) of 1-hexyl-piperazine and 20 mL of 50% aqueous sodium hydroxide. Heat the reaction for 3 hours. Add 100 mL of water and extract twice with 200 mL of ether. Combine the organic layers and dry over Na2SO4. Remove the drying agent by filtration and evaporate the solvent in vacuo to obtain the title compound. remove the heat source Heat the reaction for 3 hours extract twice with 200 mL of ether dry over Na2SO4 Remove the drying agent by filtration evaporate the solvent in vacuo