2-(chloromethyl)piperidine;hydrochloride

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

Procedure: A mixture of 170.1 g (1.0 mole) of 2-(chloromethyl)piperidine hydrochloride (M. Rink and H. G. Liem, Arch. Pharm. 292, 165-169 (1959)), 506 g (5.0 mole) of dipropylamine and 1.7 1 of dichloromethane were boiled under reflux for 3 hours, then evaporated in vacuo, and the residue was made alkaline with potassium hydroxide solution with external ice cooling. Exhaustive extraction with t-butyl methyl ether was carried out, and the combined extracts were washed twice with 100 ml of water each time, dried over sodium sulphate, and the solvent was removed by distillation in vacuo. The residue was fractionally distilled under water pump vacuum. Colourless oil of boiling point 108-114° C. (12 mm Hg ). Yield: 108.6 g (55% of theory). under reflux for 3 hours evaporated in vacuo Exhaustive extraction with t-butyl methyl ether the combined extracts were washed twice with 100 ml of water each time dried over sodium sulphate the solvent was removed by distillation in vacuo The residue was fractionally distilled under water

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

Procedure: A mixture of 170.1 g (1.0 mole) of 2-(chloromethyl)piperidine hydrochloride (M. Rink and H. G. Liem, Arch. Pharm. 292, 165-169 (1959)), 506 g (5.0 mole) of dipropylamine and 1.7 1 of dichloromethane were boiled under reflux for 3 hours, then evaporated in vacuo, and the residue was made alkaline with potassium hydroxide solution with external ice cooling. Exhaustive extraction with t-butyl methyl ether was carried out, and the combined extracts were washed twice with 100 ml of water each time, dried over sodium sulphate, and the solvent was removed by distillation in vacuo. The residue was fractionally distilled under water pump vacuum. Colourless oil of boiling point 108-114° C. (12 mm Hg ). Yield: 108.6 g (55% of theory). under reflux for 3 hours evaporated in vacuo Exhaustive extraction with t-butyl methyl ether the combined extracts were washed twice with 100 ml of water each time dried over sodium sulphate the solvent was removed by distillation in vacuo The residue was fractionally distilled under water

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

Procedure: A mixture of 170.1 g (1.0 mole) of 2-(chloromethyl)piperidine hydrochloride (M. Rink and H. G. Liem, Arch. Pharm. 292, 165-169 (1959)), 506 g (5.0 mole) of dipropylamine and 1.7 1 of dichloromethane were boiled under reflux for 3 hours, then evaporated in vacuo, and the residue was made alkaline with potassium hydroxide solution with external ice cooling. Exhaustive extraction with t-butyl methyl ether was carried out, and the combined extracts were washed twice with 100 ml of water each time, dried over sodium sulphate, and the solvent was removed by distillation in vacuo. The residue was fractionally distilled under water pump vacuum. Colourless oil of boiling point 108-114° C. (12 mm Hg ). Yield: 108.6 g (55% of theory). under reflux for 3 hours evaporated in vacuo Exhaustive extraction with t-butyl methyl ether the combined extracts were washed twice with 100 ml of water each time dried over sodium sulphate the solvent was removed by distillation in vacuo The residue was fractionally distilled under water