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The 5-Methoxytryptamine (608-07-1) as raw material we just just just just just just just color amine derivatives have you just just just a combination of things
2014-08-04
来源：亚科官网
1, route of synthesis
5- methoxytryptamine as starting material, in catalysis of potassium carbonate and allyl chloride substitution reaction occurs, and then into the salt with hydrogen chloride, N synthesis, N- allyl -5- methoxytryptamine hydrochloride.
Synthetic routes as shown below:
2, synthetic materials and methods
Material: Inova 400 nuclear magnetic resonance spectroscopy (Varian), TENSOR-27 infrared spectrometer (BRUKER), X-4 micro melting point determination instrument (Beijing Tektronix Instrument Co. Ltd., thermometer, uncorrected) reagents used were commercially available analytical grade or chemically pure.
Methods: 1, 5- methoxytryptamine hydrochloride (4.42mol 1000g), N, 5500ml two DMF N- the 10L reactor, stirring after adding anhydrous potassium carbonate 3079g (22.3mol) 1015g (13.26mol), allyl chloride, stirring at room temperature to 18 h. The reaction liquid to 50 L, 20 L water, stir after filtration, drying at room temperature and pale brown N, N- allyl -5- methoxy primary crude 1039g, yield of 87%. Melting point (M. P.) 154 ～ 159 ℃.
②, obtained N, N- allyl -5- methoxytryptamine crude product, add 10 L of isopropanol, 50 ℃ heating the solid dissolved, adding activated carbon decolorization of 80 g 10 m in. Remove activated carbon, adding hydrochloric acid 395ML and continue to stir 30m in, placed crystallization. 12 h after filtration, drying at room temperature and N, N- allyl -5 ? methoxytryptamine hydrochloride 1 kg, white, needle like crystals (88% yield
3, rationality and maneuverability:
N two, N- dimethyl formamide (DMF) as a polar aprotic solvent, the more commonly used in the alkylation reaction of halohydrocarbon were. In the experiment of DMF instead of tetrahydrofuran in the literature, with inorganic alkali potassium carbonate instead of organic alkali in the literature was not only three, the total yield is greatly improved (yield 55% to 76% Literature) [4], and the reagent cost is greatly reduced, and avoid the tetrahydrofuran using possible danger and harm thus the utility, has higher.
In this experiment, N, N- allyl -5- methoxytryptamine salt forming reaction of the decolorization activated carbon, this is because the experiment found that if the first complete the salt forming reaction and then was purified by recrystallization, the product in the color to be by 5 ~ 6 times recrystallization to remove. Therefore in the salt prior to the decolorization treatment, can be white product disposable.
