Preparation method of n-acetyl-5-methoxytryptamine
A technology of methoxytryptamine and acetyl, which is applied in the preparation of N-acetyl-5-methoxytryptamine and the field of tryptamine preparation, can solve problems such as carcinogenicity and methylene chloride toxicity, and achieve pollution reduction or Toxic, the effect of improving sleep quality
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Embodiment 1
[0017] Take 0.5kg of 5-methoxytryptamine, suspend in absolute ethanol at 15°C, add dropwise 0.5L acetic anhydride / 5L absolute ethanol solution under stirring, keep stirring for 1 hour after dropping, and adjust with sodium hydroxide solution When the pH value reaches 6.5, add 1% (w / L) activated carbon, keep stirring for 0.5 hours, filter and decarbonize, collect the filtrate, and remove the absolute ethanol by rotary evaporation of the filtrate, collect the sample, and wash the sample twice with 1.5L water repeatedly. After 0.5 hours, filter, dry, and finely grind to obtain 0.54 kg of N-acetyl-5-methoxytryptamine. After inspection, it is a white crystalline powder, soluble in ethanol and chloroform, but insoluble in water. The melting point is 115-119°C. The absorption peak in the IR spectrum is 3081cm -1 、1620cm -1 、1587cm -1 、1489cm -1 、1176cm -1 、1023cm -1 、925cm -1 、825cm -1 、797cm -1 、303cm -1 、1629cm -1 、1555cm -1 . The purity is 99.8%.
Embodiment 2
[0019] Take 1kg of 5-methoxytryptamine, suspend in 15L of absolute ethanol at 18°C, add dropwise 1L of acetic anhydride / 10L of absolute ethanol solution under stirring, keep stirring for 2 hours after dripping, and adjust the pH with sodium hydroxide solution When the value reaches 7.0, add 1% (w / L) activated carbon, keep stirring for 1 hour, filter and decarbonize, collect the filtrate, remove the absolute ethanol by rotary evaporation of the filtrate, collect the sample, and wash the sample 4 times with 3L water repeatedly, each time 1 hours, filtered, dried, and finely ground to obtain 1.13kg of N-acetyl-5-methoxytryptamine. The present invention is a white crystalline powder, dissolved in ethanol and chloroform, and insoluble in water. The melting point is 115-119°C. The absorption peak in the IR spectrum is 3081cm -1 、1620cm -1 、1587cm -1 、1489cm -1 、1176cm -1 、1023cm -1 、925cm -1 、825cm -1 、797cm -1 、303cm -1 、1629cm -1 、1555cm -1 . The purity is 100.4%.
Embodiment 3
[0021] Take 5kg of 5-methoxytryptamine, suspend in 100L of absolute ethanol at 20°C, add dropwise 5L of acetic anhydride / 100L of absolute ethanol solution under stirring, keep stirring for 4 hours after dropping, adjust the pH with sodium hydroxide solution value to 7.5, add 2% (w / L) activated carbon, keep stirring for 2 hours, filter and decarbonize, collect the filtrate, remove absolute ethanol by rotary evaporation of the filtrate, collect the sample, and wash the sample repeatedly with 30L water 6 times, each time 2 hours, filtered, dried, and finely ground to obtain 5.58kg of N-acetyl-5-methoxytryptamine, which is a white crystalline powder, dissolved in ethanol and chloroform, but insoluble in water. The melting point is 115-119°C. The absorption peak in the IR spectrum is 3081cm -1 、1620cm -1 、1587cm -1 、1489cm -1 、1176cm -1 、1023cm -1 、925cm -1 、825cm -1 、797cm -1 、303cm -1 、1629cm -1 、1555cm -1 . The purity is 99.6%.
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