Method for synthesizing black nightshade aldehyde
A synthetic method, the technology of solanum aldehyde, applied in the field of synthesis of solanum aldehyde, can solve the problems of high cost and unfavorable industrial production, and achieve the effects of low cost, simple reduction method and high yield
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Embodiment 1
[0017] 2-(α-phenylethyl)benzimidazole methyl iodide salt was synthesized with reference to literature [Craig, J.C.; Erwuibe, N.N.Synthesis, 1981, 4, 303.]. 2-(α-phenylethyl)benzimidazole (synthesized from o-phenylenediamine and α-phenylpropionic acid, reference literature: Shi Zhen, Gu Huan. Chinese Science (B Series), 1996, 26 (5), 403.) under the action of sodium alkoxide, react with methyl iodide at reflux temperature for 18h, ethanol recrystallization promptly obtains 2-(alpha-phenylethyl) benzimidazole methyl iodide salt, productive rate 85%, Elemental analysis, calculated value (%): C53.97, H5.03, N7.41; measured value (%): C53.94, H5.09, N7.38; MS m / z: 251 (M + -I).
[0018] Under stirring, add 0.01mol 2-(α-phenylethyl)benzimidazole methyl iodide salt into 20mL ethanol solution, after adding and dissolving, lower the temperature to 0-5°C, at this temperature, separate Add 0.02mol sodium chips in batches, keep the temperature and stir for 0.5h, then slowly raise the te...
Embodiment 2
[0020] 2-(α-phenylethyl)benzoxazole ethyl bromide was synthesized with reference to Example 1.
[0021] Under stirring, add 0.01mol 2-(α-phenylethyl)benzoxazole ethyl bromide into 30mL ethanol solution, after adding and dissolving, lower the temperature to 0-5°C, at this temperature, Add 0.02mol sodium chips in batches, keep the temperature and stir for 0.5h, then slowly raise the temperature to room temperature and then stir for 0.5h, add 0.01mol sodium chips, and then reflux for 1.5 hours, add 5% aqueous hydrochloric acid to make the reaction mixture Keeping the pH value at 3-5 and the temperature at 50-60° C., stir the reaction for 1.5 h, extract with chloroform (5×30 mL), and distill off the solvent to obtain solanin. The product is a colorless liquid with a yield of 68%. The NMR, mass spectrometry, infrared and elemental analysis data are consistent with those reported in the literature.
Embodiment 3
[0023] 2-(α-phenylethyl)benzimidazole benzyl chloride was synthesized with reference to Example 1.
[0024] Under stirring, add 0.01mol 2-(α-phenylethyl)benzimidazolium benzyl chloride into 30mL ethanol solution, after adding and dissolving, lower the temperature to 0-5°C, at this temperature, separate Add 0.02mol sodium chips in batches, keep the temperature and stir for 0.5h, then slowly raise the temperature to room temperature and then stir for 0.5h, add 0.01mol sodium chips, and then reflux for 1.5 hours, add 5% hydrochloric acid aqueous solution, and keep the reaction mixture Under the condition that the pH value is 3-5 and the temperature is 50-60° C., the reaction is stirred for 1.5 h, extracted with chloroform (5×30 mL), and the solvent is evaporated to obtain solanin. The product is a colorless liquid with a yield of 62%. The NMR, mass spectrometry, infrared and elemental analysis data are consistent with those reported in the literature.
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