2-Diethylaminoethylchloride hydrochloride synthesis
- Product Name:2-Diethylaminoethylchloride hydrochloride
- CAS Number:869-24-9
- Molecular formula:C6H15Cl2N
- Molecular Weight:172.1
100-37-8
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$14.00/25mL
869-24-9
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$10.00/1g
Yield:869-24-9 98.08%
Reaction Conditions:
Stage #1:2-(Diethylamino)ethanol with thionyl chloride in dichloromethane at -10 - 35; for 2.5 h;
Stage #2: with hydrogenchloride
Steps:
Preparation of 2-diethylaminochloroethane hydrochloride:
260 g of thionyl chloride and 240 g of dichloromethane were added to a 1 L reaction flask to cool down, and a mixed solution of 120 g of diethylaminoethanol and 100 g of dichloromethane was prepared in a 500 ml beaker during the cooling process, when the temperature in the reaction flask was lowered to - 10 ° C,While maintaining the temperature in the range of -10 ° C to 20 ° C, a mixture of diethylaminoethanol and dichloromethane was added dropwise, and after the completion of the dropwise addition, the temperature was raised to 35 ° C for 2.5 h, and then the dichloromethane was concentrated and concentrated until not. After concentration, the temperature was lowered to 24 ° C. 220 g of anhydrous methanol was added to the reaction flask and heated to dissolve the solid. After the solid was completely dissolved, the ice brine was cooled to -8 ° C for 7 h.Filtering to obtain 2-diethylaminochloroethane hydrochloride wet product,After the mother liquor is collected, the methanol is continuously concentrated and recovered, and the residue is subjected to freeze crystallization for 24 hours.The mother liquor product is obtained by suction filtration, and the mother liquor product is recrystallized with methanol.The obtained 2-diethylaminochloroethane hydrochloride is dried at 55-60 ° C to obtain a dry product.The purity of the liquid phase was determined to be 99.74%, and the molar yield was 98.08%.
References:
Baoji University of Arts and Sciences;Guo Yaning CN108863811, 2018, A Location in patent:Paragraph 0019
