Preparation method of N,N-dimethylaminochloropropane hydrochloride
A technology of dimethylamino chloropropane and hydrochloride, which is used in the purification/separation of amino compounds, the preparation of amino compounds by condensation/addition reactions, organic chemistry, etc. The effect of simple process, fast reaction speed and high conversion rate
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Embodiment 1
[0029] A kind of preparation method of N,N-dimethylaminochloropropane hydrochloride, concrete steps are as follows:
[0030] 1) Put 50.0 g of allyl chloride and 150 g of toluene into the four-necked reaction flask, stir, and add the catalyst TiCl 4 0.5g, 33g of dimethylamine gas was introduced at 35°C, and the reaction was terminated after 7 hours of heat preservation at 35°C. At this time, the content of allyl chloride was ≤2% through gas phase tracking detection analysis;
[0031] 2) The reaction product in step 1) is distilled under reduced pressure, reclaims 45.2 g of toluene and unreacted vinyl chloride, washes the layers with 100 g of water, and removes the catalyst TiCl 4 (catalyst TiCl 4 soluble in the water layer), add hydrochloric acid dropwise to the organic layer, adjust the pH to 2-3, react at 95°C and reflux with water for 10 hours, drop to normal temperature, filter, and dry to obtain N,N-dimethylaminochloropropane Hydrochloride 92.1g, purity 99.2%, molar yie...
Embodiment 2
[0033] A kind of preparation method of N,N-dimethylaminochloropropane hydrochloride, concrete steps are as follows:
[0034] 1) Put 50.0 g of allyl chloride and 150 g of ethanol into the four-necked reaction flask, stir, and add the catalyst TiCl 4 1.0g, 36g of dimethylamine gas was introduced at 40°C, and the reaction was terminated after 8 hours of heat preservation at 40°C. At this time, the content of allyl chloride was ≤2% through gas phase tracking detection analysis;
[0035] 2) The reaction product in step 1) is distilled under reduced pressure, reclaims 36.4 g of toluene and unreacted vinyl chloride, washes the layers with 100 g of water, and removes the catalyst TiCl 4 (catalyst TiCl 4 soluble in the water layer), hydrogen chloride gas was passed into the organic layer, the pH was adjusted to 2-3, the reaction was carried out at 100°C and refluxed with water for 10 hours, the temperature was lowered to normal temperature, filtered, and dried to obtain N,N-dimethyla...
Embodiment 3
[0037] A kind of preparation method of N,N-dimethylaminochloropropane hydrochloride, concrete steps are as follows:
[0038] 1) Put 50.0 g of allyl chloride and 150 g of toluene into a four-necked reaction flask, stir, add 1.0 g of diatomite as a catalyst, feed 38 g of dimethylamine gas at 45°C, and keep the reaction at 45°C for 10 hours, then terminate the reaction. Follow-up detection and analysis of allyl chloride content ≤ 2%;
[0039] 2) Distill the reaction product in step 1) under reduced pressure, reclaim 42.1 g of toluene and unreacted vinyl chloride, wash with 100 g of water, and filter to remove catalyst diatomaceous earth, add hydrochloric acid dropwise to the organic layer, and adjust the pH to 2 ~3. Reaction and reflux with water at 112°C for 12 hours, lowered to room temperature, filtered, and dried to obtain 93.0 g of N,N-dimethylaminochloropropane hydrochloride with a purity of 99.1% and a molar yield of 90.0%.
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