2-chloro-N,N-bis(2-chloroethyl)ethanamine;hydrochloride

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: When all of the water of the reaction has been eliminated, 55 g of tris(2-chloroethyl)amine hydrochloride are introduced. The mixture is heated at 130° C. for 5 hours, then cooled. Excess sodium alcoholate is then neutralized with a 10% aqueous solution of hydrochloric acid. The 3-oxaheptan-1-ol is removed by distillation and the sodium chloride is removed by filtration. The desired product, tris(3,6-dioxadecyl)amine, is distilled (192° C. under 0.1 mmHg). cooled The 3-oxaheptan-1-ol is removed by distillation the sodium chloride is removed by filtration The desired product, tris(3,6-dioxadecyl)amine, is distilled (192° C. under 0.1 mmHg)

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

実験手順: To the mixture thus obtained, 51.6 g of tris(2-chloroethyl)amine hydrochloride (0.215 mole) are added. The mixture is then heated at the reflux temperature of the 2-methoxyethanol (125° C.) for 12 hours and then the solvent is removed by distillation under reduced pressure. The excess sodium 2-methoxyethanolate is neutralized by the addition of 11.6 cm3 aqueous HCl (10 N). The sodium chloride is filtered off and the solution is distilled. To the mixture thus obtained the solvent is removed by distillation under reduced pressure The excess sodium 2-methoxyethanolate is neutralized by the addition of 11.6 cm3 aqueous HCl (10 N) The sodium chloride is filtered off the solution is distilled

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: When all of the water of the reaction has been eliminated, 55 g of tris(2-chloroethyl)amine hydrochloride are introduced. The mixture is heated at 130° C. for 5 hours, then cooled. Excess sodium alcoholate is then neutralized with a 10% aqueous solution of hydrochloric acid. The 3-oxaheptan-1-ol is removed by distillation and the sodium chloride is removed by filtration. The desired product, tris(3,6-dioxadecyl)amine, is distilled (192° C. under 0.1 mmHg). cooled The 3-oxaheptan-1-ol is removed by distillation the sodium chloride is removed by filtration The desired product, tris(3,6-dioxadecyl)amine, is distilled (192° C. under 0.1 mmHg)

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

実験手順: To the mixture thus obtained, 51.6 g of tris(2-chloroethyl)amine hydrochloride (0.215 mole) are added. The mixture is then heated at the reflux temperature of the 2-methoxyethanol (125° C.) for 12 hours and then the solvent is removed by distillation under reduced pressure. The excess sodium 2-methoxyethanolate is neutralized by the addition of 11.6 cm3 aqueous HCl (10 N). The sodium chloride is filtered off and the solution is distilled. To the mixture thus obtained the solvent is removed by distillation under reduced pressure The excess sodium 2-methoxyethanolate is neutralized by the addition of 11.6 cm3 aqueous HCl (10 N) The sodium chloride is filtered off the solution is distilled

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

実験手順: To the preceding mixture, 51.6 g tris-(2-chloroethyl)amine hydrochloride (0.215 mole) were added. The mixture was then heated under reflux of the 2-methoxyethanol (θ=125° C.) for 12 hours and the solvent distilled off under reduced pressure. The excess sodium 2-methoxyethanolate was neutralized by addition of 11.6 cm3 of aqueous (10 N) HCl. The sodium chloride was filtered and the solution distilled. The mixture was then heated the solvent distilled off under reduced pressure The excess sodium 2-methoxyethanolate was neutralized by addition of 11.6 cm3 of aqueous (10 N) HCl The sodium chloride was filtered the solution distilled

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

実験手順: 51.6 g (i.e., 0.215 mol) of tris-(2-chloroethyl)-amine hydrochloride were added to the above mixture (a). The mixture was subsequently heated at the reflux temperature of the 2-methoxyethanol (125° C.) for 12 hours and the solvent was then distilled under reduced pressure. The excess sodium 2-methoxyethanolate was neutralized by adding 11.6 cm3 of aqueous HCl (10 N) thereto. The sodium chloride was filtered off and the solution was distilled. the solvent was then distilled under reduced pressure by adding 11.6 cm3 of aqueous HCl (10 N) The sodium chloride was filtered off the solution was distilled

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

実験手順: 51.6 g (i.e., 0.215 mol) of tris-(2-chloroethyl)-amine hydrochloride were added to the above mixture (a). The mixture was subsequently heated at the reflux temperature of the 2-ethoxyethanol for 12 hours and the solvent was then distilled under reduced pressure. The excess sodium 2-ethoxyethanolate was neutralized by adding 12 cm3 of aqueous HCl (10 N) thereto. The sodium chloride was filtered off and the solution was distilled. The tris-(3,6-dioxaoctyl)-amine distilled between 200° C. and 210° C. under a pressure of 1 mm Hg. The yield was 68%. the solvent was then distilled under reduced pressure by adding 12 cm3 of aqueous HCl (10 N) The sodium chloride was filtered off the solution was distilled The tris-(3,6-dioxaoctyl)-amine distilled between 200° C. and 210° C. under a pressure of 1 mm Hg

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

実験手順: 51.6 g (namely, 0.215 mol) of tris-(2-chloroethyl)-amine hydrochloride were added to the above mixture. The mixture was subsequently heated at the reflux temperature of the 2-methoxyethanol (125° C.) for 12 hours and the solvent was then distilled under reduced pressure. The excess sodium 2-methoxyethanolate was neutralized by adding 11.6 cm3 of aqueous HCl (10 N). The sodium chloride was filtered off and the solution was distilled. the solvent was then distilled under reduced pressure by adding 11.6 cm3 of aqueous HCl (10 N) The sodium chloride was filtered off the solution was distilled

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

実験手順: 51.6 g (namely, 0.215 mol) of tris-(2-chloroethyl)-amine hydrochloride were added to the above mixture. The mixture was subsequently heated at the reflux temperature of the 2-methoxyethanol (125° C.) for 12 hours and the solvent was then distilled under reduced pressure. The excess sodium 2-ethoxyethanolate was neutralized by adding 11.6 cm3 of aqueous HCl (10 N). The sodium chloride was filtered off and the solution was distilled. the solvent was then distilled under reduced pressure by adding 11.6 cm3 of aqueous HCl (10 N) The sodium chloride was filtered off the solution was distilled

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: When all of the water of the reaction has been eliminated, 55 g of tris(2-chloroethyl)amine hydrochloride are introduced. The mixture is heated at 130° C. for 5 hours, then cooled. Excess sodium alcoholate is then neutralized with a 10% aqueous solution of hydrochloric acid. The 3-oxaheptan-1-ol is removed by distillation and the sodium chloride is removed by filtration. The desired product, tris(3,6-dioxadecyl)amine, is distilled (192° C. under 0.1 mmHg). cooled The 3-oxaheptan-1-ol is removed by distillation the sodium chloride is removed by filtration The desired product, tris(3,6-dioxadecyl)amine, is distilled (192° C. under 0.1 mmHg)

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

実験手順: To the mixture thus obtained, 51.6 g of tris(2-chloroethyl)amine hydrochloride (0.215 mole) are added. The mixture is then heated at the reflux temperature of the 2-methoxyethanol (125° C.) for 12 hours and then the solvent is removed by distillation under reduced pressure. The excess sodium 2-methoxyethanolate is neutralized by the addition of 11.6 cm3 aqueous HCl (10 N). The sodium chloride is filtered off and the solution is distilled. To the mixture thus obtained the solvent is removed by distillation under reduced pressure The excess sodium 2-methoxyethanolate is neutralized by the addition of 11.6 cm3 aqueous HCl (10 N) The sodium chloride is filtered off the solution is distilled