heptan-2-amine

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

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

Procedure: 36.5 g (0.2 mol) of 2,3,5,6-tetramethylbenzyl chloride, 46.0 g (0.4 mol) of 2-aminoheptane and 100 ml of benzene are refluxed for 2 hours. The solvent is then removed in vacuo. A solution of 8 g (0.2 mol) of sodium hydroxide in methanol is then added to the residue to liberate the free base. The reaction product is separated from the precipitated sodium chloride by means of a suction filter, and the excess of 2-aminoheptane is removed by vacuum distillation. The 2-(2,3,5,6-tetramethylbenzyl)aminoheptane obtained is then treated with ethereal hydrochloric acid to convert it into the hydrochloride which is recrystallised from methanol/ethyl acetate. The melting point of the hydrochloride is 155° C. The solvent is then removed in vacuo The reaction product is separated from the precipitated sodium chloride by means of a suction filter the excess of 2-aminoheptane is removed by vacuum distillation

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

Procedure: 100 ml of methanol and 100 mmol of 2-heptylamine are initially taken and 100 mmol of benzaldehyde are added dropwise at 24° C. in the course of 15 minutes. Stirring is effected for 6 hours at 24° C., the completeness of the iminization is checked by GC, 0.5 g of Pd/C (10% by weight) is added and the crude mixture is hydrogenated with hydrogen for 5 hours at atmospheric pressure. A sample is taken and the composition is investigated by GC analysis. is added

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

Procedure: The equipment, procedure and reactants were the same as in Example 31 with the exception that 10.01 g (0.07 mole) of n-hexylisothiocyanate, 8.05 g (0.07 mole) 2-aminoheptane, 35 ml ethanol 2B, 11.7 g (0.075 mole) ethyl iodide, 200 ml of toluene and a one percent solution sodium hydroxide (0.08 mole) were used as reactants and reagents in the procedure. The reaction produced 19.6 g (98 weight percent of theory yield of a clear liquid having a nD30 of 1.4765. The product was identified as the title product by IR and NMR spectra analyses. The reaction produced 19.6 g (98 weight percent of theory yield of a clear liquid

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

Procedure: The equipment was the same as in Example 26 above. 11.5 g (0.1 mole) 2-aminoheptane was mixed with 50 ml ethanol 2B and 15.7 g (0.1 mole) N-heptyl isothiocyanate was added, resulting in an exothermic reaction during which the temperature rose from 25° to 65° C. The reaction mixture was refluxed on a steam bath for 1.5 hours. 17.16 g (0.11 mole) ethyl iodide was then added to the thiourea and the mixture refluxed for 1.5 hours on a steam bath. The product was vacuum evaporated to produce 44.0 g of an isothiuronium salt. The isothiuronium salt was dissolved in 200 ml of toluene and washed with 100 cc of 5 percent sodium hydroxide. The toluene layer was then washed twice with 150 cc portions of water, dried over magnesium sulfate, filtered and vacuum evaporated. The product was then stripped under high vacuum to produce 7.78 g (92.6 weight percent of theory yield) of a clear, yellow liquid having a nD30 of 1.4768. The product was identified as the title product by IR and NMR spectra analyses. was added resulting in an exothermic reaction during which the temperature rose from 25° to 65° C The reaction mixture was refluxed on a steam bath for 1.5 hours the mixture refluxed for 1.5 hours on a steam bath evaporated

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

Procedure: The equipment was the same as in Example 26 above. 11.5 g (0.1 mole) 2-aminoheptane was mixed with 50 ml ethanol 2B and 15.7 g (0.1 mole) N-heptyl isothiocyanate was added, resulting in an exothermic reaction during which the temperature rose from 25° to 65° C. The reaction mixture was refluxed on a steam bath for 1.5 hours. 17.16 g (0.11 mole) ethyl iodide was then added to the thiourea and the mixture refluxed for 1.5 hours on a steam bath. The product was vacuum evaporated to produce 44.0 g of an isothiuronium salt. The isothiuronium salt was dissolved in 200 ml of toluene and washed with 100 cc of 5 percent sodium hydroxide. The toluene layer was then washed twice with 150 cc portions of water, dried over magnesium sulfate, filtered and vacuum evaporated. The product was then stripped under high vacuum to produce 7.78 g (92.6 weight percent of theory yield) of a clear, yellow liquid having a nD30 of 1.4768. The product was identified as the title product by IR and NMR spectra analyses. was added resulting in an exothermic reaction during which the temperature rose from 25° to 65° C The reaction mixture was refluxed on a steam bath for 1.5 hours the mixture refluxed for 1.5 hours on a steam bath evaporated

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

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

Procedure: The equipment, procedure and reactants were the same as in Example 31 with the exception that 10.01 g (0.07 mole) of n-hexylisothiocyanate, 8.05 g (0.07 mole) 2-aminoheptane, 35 ml ethanol 2B, 11.7 g (0.075 mole) ethyl iodide, 200 ml of toluene and a one percent solution sodium hydroxide (0.08 mole) were used as reactants and reagents in the procedure. The reaction produced 19.6 g (98 weight percent of theory yield of a clear liquid having a nD30 of 1.4765. The product was identified as the title product by IR and NMR spectra analyses. The reaction produced 19.6 g (98 weight percent of theory yield of a clear liquid

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

Procedure: The equipment was the same as in example 26 above. 11.5 g (0.1 mole) 2-aminoheptane was mixed with 50 ml ethanol 2B and 15.7 g (0.1 mole) N-heptyl isothiocyanate was added, resulting in an exothermic reaction during which the temperature rose from 25° to 65° C. The reaction mixture was refluxed on a steam bath for 1.5 hours. 17.16 g (0.11 mole) ethyl iodide was then added to the thiourea and the mixture refluxed for 1.5 hours on a steam bath. The product was vacuum evaporated to produce 44.0 g of an isothiuronium salt. The isothiuronium salt was dissolved in 200 ml of toluene and washed with 100 cc of 5 percent sodium hydroxide. The toluene layer was then washed twice with 150 cc portions of water, dried over magnesium sulfate, filtered and vacuum evaporated. The product was then stripped under high vacuum to produce 7.78 g (92.6 weight percent of theory yield) of a clear, yellow liquid having a nD30 of 1.4768. The product was identified as the title product by IR and NMR spectra analyses. was added resulting in an exothermic reaction during which the temperature rose from 25° to 65° C The reaction mixture was refluxed on a steam bath for 1.5 hours the mixture refluxed for 1.5 hours on a steam bath evaporated