Method for synthesizing diindolylmethane derivative

Abstract

The invention discloses a method for synthesizing a diindolylmethane derivative. The method comprises the following steps of: a, preparing an acid-modified H beta molecular sieve; b, putting the acid-modified H beta molecular sieve into a fixed bed reactor, mixing indol and benzaldehyde or benzaldehyde with a substituent group according to a molar ratio of (3.5-5):1, dissolving into lower alcohol, and introducing into the fixed bed reactor at the speed of between 0.5 and 2 mL / minute to react continuously; and c, adding water into liquid flowing out of the reactor, stirring, standing for precipitating, filtering, and drying a filter material. By the method, the synthesized product has high quality and yield and low cost, the process time is shortened greatly, and a synthetic process is simple and convenient and is easy to operate.

Description

technical field [0001] The present invention relates to the synthetic method of compound, specifically relates to the new synthetic method of diindolylmethane derivative. Background technique [0002] Diindolylmethane and its derivatives are a very important class of indole derivatives, which have many important biological activities. For example, diindolylmethane derivatives have anticancer activity, and can be used to inhibit the growth of bladder cancer, renal cell carcinoma and breast tumors, and also have inhibitory effects on lung cancer and prostate cancer. Diindolylmethane derivatives also have analgesic, tranquilizing, etc. effect. In addition, diindolylmethane derivatives are also important fine chemical raw materials, which can be used in dyes, sensors and other fields. [0003] At present, the synthesis methods of diindolylmethane derivatives usually adopt batch methods, but these methods all have the disadvantages of long reaction time, high energy consumption...

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Problems solved by technology

[0003] At present, the synthesis methods of diindolylmethane derivatives usually adopt batch methods, but these methods have the disadvantages of long reaction time, high energy consumption, difficult reaction control, unstable product quality, and low synthesis efficiency.

For example, Synthesis 5 (2001) 783-787 reported a method using Lewis acid LiClO 4 Catalyze indole and benzaldehyde reaction 5h, generate the method for phenyl diindolylmethane (yield is 90%), the Lewis acid in this method is harmful to environment, and the post-reaction treatment is complicated; Synthetic Communications 33(2003) 3687- 3694 reported a kind of dichloromethane as solvent, under the catalysis of HY molecular sieve, reacted for 1h, indole and aldehyde had electrophilic substitution reaction to generate phenyl diindolylmethane method (yield was 85%), the method There is a large amount of solvent pollution and the disadvantages that the reaction is not easy to control; Catalysis Communications 5 (2004) 371-375 reported that a kind of dichloromethane was also used as a solvent and reacted for 2 hours under the catalysis of metal zinc-modified HY molecular sieve. Indole and benzene Formaldehyde reaction generates the method (yield is 85%) of phenyldiindolylmethane, and this method exists solvent pollution equally, and the shortcoming that reaction is difficult to control; The batch method of methyl n-hexylimidazole catalyzing the reaction of indole and aldehydes, the reaction time is 1h (yield is 97%), the ionic liquid catalyst in this method is difficult to prepare, expensive, and the post-reaction treatment process is complicated

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