3,4-methylenedioxyphenethylamine hydrochloride-5-chlorosalicylaldehyde, synthesis method and application of 3,4-methylenedioxyphenethylamine hydrochloride-5-chlorosalicylaldehyde
A technology of piperonyl ethylamine and chlorosalicylaldehyde, which is applied in the field of medicine, can solve problems such as the synthesis and activity research of new Schiff bases that have not yet been seen, and achieve good medicinal value, mild reaction conditions, and low-cost reaction raw materials. Effect
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Embodiment 1
[0023] Dissolve 0.01mol of 5-chlorosalicylaldehyde and 0.01mol of piperethylamine in 30mL of absolute ethanol (use Molecular sieve dehydration), the resulting liquid was refluxed and reacted at 78°C under stirring conditions until complete (TLC tracking detection, about 3h), after the reaction was stopped, the reaction liquid was fully cooled to 15°C, and stood for 6h, and yellow needle-shaped crystals were precipitated. After filtration, the obtained crystals were vacuum-dried at room temperature for 6 h to obtain a yellow solid product with a yield of 90%.
[0024] The yellow solid product obtained above was subjected to infrared spectrum, ultraviolet spectrum, 1 H and 13 C nuclear magnetic resonance spectrum and electrospray mass spectrometry identification, their spectra are as follows figure 1 , 2 , 3, 4 and 5, the specific spectral characteristics are as follows:
[0025] Infrared spectrum: (KBr,cm -1 )3440(ν N-H ), 2912, 2846 (ν Ar-H ),1637(ν C=N ),1484(ν C=C ...
Embodiment 2
[0033] Take 0.01mol of 5-chlorosalicylaldehyde and 0.01mol of piperethylamine and mix and dissolve in 100mL of dichloromethane (use the dichloromethane before use) Molecular sieve dehydration), the obtained solution was stirred and reacted at 45°C until complete (TLC tracking detection, about 12h), after the reaction was stopped, most of the dichloromethane solvent (accounting for 90% of the amount of dichloromethane used) was distilled off under reduced pressure, and the remaining reaction The liquid was fully cooled to 10° C., left standing for 12 hours, yellow needle-like crystals were precipitated, filtered, and the obtained crystals were dried in vacuum at room temperature for 2 hours to obtain a yellow solid product with a yield of 75%.
[0034] The above-mentioned yellow solid product was subjected to spectroscopic analysis, and its spectral characteristics were the same as those obtained in Example 1. Therefore, it was determined that the yellow solid product prepared ...
Embodiment 3
[0036] Mix and dissolve 0.01mol of 5-chlorosalicylaldehyde and 0.01mol of piperethylamine in 200mL of chloroform / anhydrous methanol mixed solvent (the volume ratio of chloroform and anhydrous methanol is 1:1, and the use of chloroform and anhydrous methanol used before Molecular sieve dehydration), the obtained solution was stirred and reacted at 60°C until complete (TLC tracking detection, about 1h), after the reaction was stopped, most of the solvent was removed by vacuum distillation (accounting for 90% of the organic solvent), and the remaining reaction solution was fully Cool to room temperature 25°C, let stand for 1 h, precipitate yellow needle-like crystals, filter, and vacuum-dry the obtained crystals at room temperature for 24 h to obtain piperonyl ethylamine 5-chlorosalicylaldehyde with a yield of 70%.
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