Method for preparing biferrocenyl chalcone
A technology of base chalcone and ferrocene, which is applied in the field of preparation of ferrocene base chalcone, can solve the problems such as cumbersome operation of monoacetyl ferrocene, and achieve the effect of high-purity preparation
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Embodiment 1
[0028] In the first step, add substituted phenylacrylic acid and phosphorus pentachloride to the reactor, heat to 20-100°C, stir for 1-5 hours, and the molar ratio of substituted phenylacrylic acid and phosphorus pentachloride is 1: (1-2) ;
[0029] In the second step, add solvent, ferrocene and Lewis acid to the reactor, heat to 25 ℃ ~ the temperature of reflux in the reactor, react for 0.5 ~ 3h, the number of milliliters of solvent added is the number of moles of substituted phenylacrylic acid 150-845 times, the molar ratio of substituted phenylacrylic acid and ferrocene is 1: (0.5-0.83), the molar ratio of substituted phenylacrylic acid and Lewis acid is 1: (0.5-2.5);
[0030] In the 3rd step, the solvent added in the second step is evaporated under reduced pressure, and the remaining solid is added in water, and the milliliter number of adding water is more than 550 times of the molar number of ferrocene added in the second step, and sodium bicarbonate is added to no more ...
Embodiment 2
[0035] In the first step, add 0.01mol cinnamic acid and 0.012mol phosphorus pentachloride to the reactor, heat to 20°C and stir for 2 hours;
[0036] In the second step, add 4.8ml of carbon disulfide, 0.008mol of ferrocene, and 0.01mol of anhydrous aluminum chloride to the reactor, heat it to 45°C and keep it warm for 3 hours;
[0037] The third step is to remove carbon disulfide by steaming under reduced pressure, add 5.5ml of water to the remaining solid, and then add sodium bicarbonate until no more bubbles are generated, then filter, and the filtered solid is first washed with 5% hydrochloric acid by mass fraction, and then washed with 5% hydrochloric acid by mass fraction Wash with 5% sodium hydroxide, and finally wash with water until the filtrate is neutral to obtain 2.17g of a purple solid, which is ferrocenylchalcone, with a yield of 86%; Waters company, model: 600E; Chromatographic column specification: Venusil-MP C18 chromatographic column, carbon load: 18%, particl...
Embodiment 3
[0039] In the first step, add 0.01mol cinnamic acid and 0.016mol phosphorus pentachloride to the reactor, heat to 50°C and stir for 3.5h;
[0040] In the second step, add 6ml of carbon disulfide, 0.005mol of ferrocene, and 0.015mol of anhydrous zinc chloride to the reactor, heat to 70°C and keep it warm for 2 hours;
[0041] The third step is to remove carbon disulfide by steaming under reduced pressure, add 11ml of water to the remaining solid, then add sodium bicarbonate until no bubbles are produced, then filter, and the filtered solid is first washed with 10% hydrochloric acid with a mass fraction of Wash with 10% sodium hydroxide, and finally wash with water until the filtrate is neutral to obtain 1.33g of purple-red solid as ferrocenylchalcone, with a yield of 84%; its purity detected by high performance liquid chromatography is: 94% .
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