Method for synthesizing benzyldimethyl[3-(myristamide)propyl]ammonium chloride
A technology of benzyl dimethyl and myristyl amido, which is applied in the field of synthesis of Michaelis antibacterial drug propyl]ammonium chloride, can solve the problem of high requirements for residual solvent control, high requirements for reaction equipment, and relatively high environmental impact. Major problems, to achieve the effect of easy control of product quality, simplified operation, and reduced 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), 1.2 8(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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