We will provide a detailed introduction to the reaction results using a flow-type microwave synthesis device!
Our "flow-type microwave synthesis device" can heat the entire system while flowing the target substance (liquid) through a glass serpentine tube, eliminating the need for multiple heating steps and allowing for uniform heating. Using this device, we will introduce the reaction results of producing tetrahydrocarbazole through the Fischer indole synthesis reaction of phenylhydrazine and cyclohexanone, as well as the experimental methods. [Overview] ■ Production of tetrahydrocarbazole through the Fischer indole synthesis reaction of phenylhydrazine and cyclohexanone. *For more details, please refer to the PDF document or feel free to contact us.
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【Experimental Method Details】 - Cyclohexanone was mixed with acetic acid to achieve a concentration of 2.0M, forming solution A. - Phenylhydrazine was dissolved in acetonitrile to achieve a concentration of 2.2M, forming solution B. - Solutions A and B were connected to pumps and fed into a 200W machine at a flow rate of 7.5 mL/min each (total 15 mL/min). - Microwave irradiation was applied, and after about 5 minutes, it was confirmed that the temperature stabilized (at 240°C), and the reaction solution was collected for 1 hour. - The collected reaction solution was allowed to stand in the refrigerator for 3 hours, after which the precipitated product (tetrahydrocarbazole) was filtered out (52.6 g). - The filtrate was concentrated, then dissolved in ethyl acetate, washed with brine, and the organic layer was dried with MgSO4. - After removing the drying agent by filtration, the filtrate was concentrated, and recrystallization was performed using acetonitrile, yielding an additional 47.1 g of product. - The filtrate was concentrated and purified by silica gel column chromatography (n-hexane/EtOAc = 10/1), recovering 15.3 g of product. *For more details, please refer to the PDF document or feel free to contact us.*
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【Purpose】 ■ For researchers in basic cosmetics and pharmaceuticals *For more details, please refer to the PDF document or feel free to contact us.*
Company information
Sida FDS Co., Ltd. was established as the development division of the Sida Group, which consistently engages in "monozukuri" (manufacturing) to meet customer needs, from machining parts for machine tools and industrial machinery to the assembly of complete systems. Our goal is to develop and sell products that can be patented, not only in Japan but also globally. Moving forward, we aim to be a manufacturer that is needed by society through the development of our own products (such as environmental evaluation testing equipment and microwave irradiation devices for chemical applications).
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