Method for synthesizing benzyldimethyl[3-(myristamide)propyl]ammonium chloride
A benzyl dimethyl and myristyl amide group technology is applied in the synthesis field of Mie's antibacterial drug propyl] ammonium chloride), which can solve the problem of high residual solvent control requirements, high reaction equipment requirements, and relatively high environmental impact. It can easily control the product quality, simplify the operation, and reduce the toxicity.
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[0025] (1) Add N,N-dimethylpropylenediamine (31.0g, 0.303mol), 600ml ethyl acetate and triethylamine (31.0g, 0.306mol) to a 1000ml round bottom bottle, and add dropwise under stirring Myristoyl chloride (73.8 g, 0.299 mol). After the addition was complete, the reaction was heated to reflux for 3 hours and cooled to room temperature. The precipitated white solid was filtered off, and ethyl acetate was concentrated under reduced pressure to dryness to obtain a white solid. Add 250ml of petroleum ether at 60-90°C for recrystallization to obtain 72.2g of 3-myristoylamino-N,N-dimethylpropylamine as a white solid with a yield of 77.4% based on myristoyl chloride and a melting point of 51-52°C .
[0026] 1 H NMR (CDCl 3 )δ: 0.88(t, 3H), 1.28(m, 20H), 1.63(m, 4H), 2.14(t, 2H), 2.23(s, 6H), 2.37(t, 2H), 3.34(q, 2H ), 6.94 (br, 1H).
[0027] (2) Add 3-myristamido-N, N-dimethylpropylamine (62.4g, 0.20mol, 750ml ethyl acetate to a 2000ml round bottom bottle, add benzyl chloride (34....
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