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ChemicalBook CAS DataBase List 3-Chloro-1-(N,N-dimethyl)propylamine
109-54-6

3-Chloro-1-(N,N-dimethyl)propylamine synthesis

8synthesis methods
3-(DIMETHYLAMINO)PROPYL CHLORIDE HYDROCHLORIDE

5407-04-5

3-Chloro-1-(N,N-dimethyl)propylamine

109-54-6

General procedure for the synthesis of 3-chloro-1-(N,N-dimethyl)propylamine from N,N-dimethylaminopropyl chloride hydrochloride: flake solid NaOH (42.1 g, 1052.5 mmol, 1.0 eq.) was dissolved in 142.1 g of water, a process which is exothermic, and an aqueous NaOH solution was obtained and then cooled down to 30 °C. In a 500 mL two-neck flask, HCl (104 g, 658 mmol, 1.0 eq.) and the above aqueous NaOH solution were added, the temperature was raised to 45 °C and the reaction was started with continuous stirring for 2 hours. After completion of the reaction, the reaction solution was cooled to room temperature (30 °C). The organic layer was separated and collected to give 74.93 g of wet 3-chloro-1-(N,N-dimethyl)propylamine (CPA). The water content of the product was determined to be 2.755% and the yield was 91.07% (as anhydrous CPA).

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Yield:109-54-6 91.07%

Reaction Conditions:

with sodium hydroxide in water at 45; for 2 h;

Steps:

3

The flaky solid NaOH (42.1 g, 1052.5 mmol, 1.0 equiv.) was dissolved in 142.1 g of water, a large amount of heat was released to give an aqueous solution of NaOH, which was cooled to 30 ° C. A solution of CPA.HCl (104 g, 658 mol, 1.0 equiv.) and the above aqueous solution of NaOH was added to a 500 mL two-necked flask and the temperature was raised to 45 ° C and the reaction was started and stirred for 2 h.
Reaction post-treatment:
The reaction solution was cooled to room temperature (30 ° C). The organic layer was separated and collected, and 74.93 g of wet CPA was obtained. The water content was found to be 2.755% and the yield was 91.07% (excluding moisture in the CPA).

References:

CN105294496,2016,A Location in patent:Paragraph 0128; 0129; 0130; 0131; 0132

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