A kind of synthetic method of glabridin
A technology of glabridin and its synthesis method, which is applied in the direction of organic chemistry, can solve the problems of long cycle time, and achieve the effects of high total yield, rapid and efficient synthesis, and cheap and easy-to-obtain raw materials
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[0025] 1. Add 0.30g (1.85mmol) of 7-hydroxycoumarin into a 10mL round bottom flask, add 3mL of acetonitrile, 0.31mL (2.04mmol) of DBU and 0.32mg (0.00185mmol) of copper chloride dihydrate in turn, at 0°C Slowly add 0.22mL (1.94mmol) 3-chloro-3-methyl-1-butyne, react at room temperature for 10h, TLC monitors the complete reaction of raw materials. Pour the reaction solution into saturated NaHCO 3 In aqueous solution, after extraction with ethyl acetate, over anhydrous MgSO 4 Dry, filter, concentrate under reduced pressure, and separate by column chromatography (eluent: EA / PE=1:3) to obtain compound I (0.37g, yield 90%, white solid, Mp: 253-255°C), reaction equation As follows:
[0026]
[0027] The structural characterization data of the obtained compound I are: 1 H NMR (400MHz, CDCl 3 )δ7.64(d, J=9.2Hz, 1H), 7.36(d, J=8.8Hz, 1H), 7.32(d, J=2.0Hz, 1H), 7.04(dd, J=8.4, 2.0Hz, 1H), 6.28(d, J=9.6Hz, 1H), 2.66(s, 1H), 1.71(s, 6H); HRMS(ESI) m / z: theoretical value C 14 h 1...
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