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ChemicalBook CAS DataBase List 3-(DIMETHYLAMINO)PROPYL CHLORIDE HYDROCHLORIDE
5407-04-5

3-(DIMETHYLAMINO)PROPYL CHLORIDE HYDROCHLORIDE synthesis

4synthesis methods
-

Yield:5407-04-5 90%

Reaction Conditions:

with diatomaceous earth in toluene at 45; for 10 h;Reagent/catalyst;Temperature;Solvent;

Steps:

1-3 Example 3
A preparation method of N,N-dimethylaminochloropropane hydrochloride, the specific steps are as follows:1) Put 50.0 g of chloropropene and 150 g of toluene into a four-port reaction flask, and stir.Add 1.0g of diatomite as catalyst, and 38g of dimethylamine gas at 45.After holding the reaction at 45 for 10h, the reaction is terminated. At this time, the gas phase tracking detection analysis analyzes the content of chloropropene ≤ 2%;2) The reaction product in step 1) is distilled under reduced pressure, and 42.1 g of toluene and unreacted vinyl chloride are recovered, washed with 100 g of water, and filtered to remove the catalyst diatomaceous earth. Hydrochloric acid is added dropwise to the organic layer to adjust the pH to 2 3. Reaction and reflux with water at 112 for 12h, lower to normal temperature, filter and dry to obtain 93.0g of N,N-dimethylaminochloropropane hydrochloride, purity 99.1%, molar yield 90.0%.

References:

Henan Yuchen Pharmaceutical Co., Ltd.;Li Shanshan;Wei Liqiang;Zhang Yuanfeng;Cheng Lihong;Luo Ming;Zhou Jinlong;Zhang Ying CN111153807, 2020, A Location in patent:Paragraph 0028-0039

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