A kind of method that o-ethylaniline dehydrocyclization prepares indole
A technology of o-ethylaniline and dehydrocyclization, which is applied in the field of indole production, can solve the problems of high reaction temperature, easy loss, and high production cost, and achieve the effects of low reaction temperature, easy operation, and high selectivity
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Embodiment 1
[0019] In a 0.5L autoclave equipped with a gas-liquid separator, add 300 milliliters of o-ethylaniline, catalyst RU-Al 2 o 3 8.64 grams, wherein the content of Ru is 3%, 0.86 grams of boric acid, replaced by nitrogen, heated up to 280 ° C, when the pressure in the kettle is 0.5Mpa, slowly release the pressure, and keep the reaction temperature when the pressure in the kettle reaches 0.3Mpa Continue to release the pressure slowly, so many times until the pressure in the kettle is lower than 0.1Mpa, after the reaction is completed, the material is cooled and cooled, and the ice-water cooling product indole is separated out from the solution. The conversion rate of o-ethylaniline is above 72%, the yield of indole is above 45%, and the selectivity of indole is above 65%.
Embodiment 2
[0021] In a 0.5L autoclave equipped with a gas-liquid separator, add 300 milliliters of o-ethylaniline, catalyst RU-Al 2 o 3 17.3 grams, wherein the content of Ru is 3%, 1.73 grams of boric acid, replaced by nitrogen, heated to 300 ° C, when the pressure in the kettle is 0.5Mpa, slowly release the pressure, and keep the reaction temperature when the pressure in the kettle reaches 0.3Mpa Continue to release the pressure slowly, so many times until the pressure in the kettle is lower than 0.1Mpa, after the reaction is completed, the material is cooled and cooled, and the ice-water cooling product indole is separated out from the solution. The conversion rate of o-ethylaniline is above 75%, the yield of indole is above 50%, and the selectivity of indole is above 70%.
Embodiment 3
[0023] In a 0.5L autoclave equipped with a gas-liquid separator, add 300 milliliters of o-ethylaniline, catalyst RU-Al 2 o 3 14.4 grams, wherein the content of Ru is 8%, boric acid 1.44 grams, nitrogen displacement, heating up to 380 ° C, when the pressure in the kettle is 0.5Mpa, slowly release the pressure, and keep the reaction temperature after the pressure relief. When the pressure in the kettle reaches 0.3Mpa Continue to release the pressure slowly, so many times until the pressure in the kettle is lower than 0.1Mpa, after the reaction is completed, the material is cooled and cooled, and the ice-water cooling product indole is separated out from the solution. The conversion rate of o-ethylaniline is above 90%, the yield of indole is above 80%, and the selectivity of indole is above 92%.
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