Preparation method of indole-3-methanol
A technology for indole and methanol, applied in the field of preparation of indole-3-methanol, can solve the problems of difficult separation of reducing agents, increase in preparation cost and high preparation cost, achieve easy separation and regeneration, reduce preparation cost and improve reaction degree Effect
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Embodiment 1
[0026] Indole-3-carbinol was synthesized according to the following steps:
[0027] (1) Add dichloromethane into the reaction flask in the ice-water bath under the protection of nitrogen, start stirring, add zirconium chloride, then add tetrahydrofuran dropwise within 30 minutes, continue stirring for 1 hour, then add diethylamine and cyclopentadiene , the mass ratio of dichloromethane, zirconium chloride, tetrahydrofuran, diethylamine, and cyclopentadiene is 2.47:1.45:3.87:1:1.02, continue stirring for 2 hours, then heat to 45°C for reflux reaction for 7 hours, and cool to room temperature Afterwards, the product obtained is suction filtered, the filter cake is repeatedly washed with formic acid and then suction filtered again, and the obtained filter cake is recrystallized with chloroform to obtain zirconocene dichloride;
[0028] (2) Add montmorillonite to distilled water, heat to 70°C and stir for 10 minutes to obtain a montmorillonite solution with a concentration of 1.25...
Embodiment 2
[0034] Indole-3-carbinol was synthesized according to the following steps:
[0035] (1) Add dichloromethane into the reaction flask in the ice-water bath under the protection of nitrogen, start stirring, add zirconium chloride, then add tetrahydrofuran dropwise within 30 minutes, continue stirring for 1 hour, then add diethylamine and cyclopentadiene , the mass ratio of dichloromethane, zirconium chloride, tetrahydrofuran, diethylamine, and cyclopentadiene is 2.47:1.45:3.87:1:1.02, continue stirring for 2 hours, then heat to 45°C for reflux reaction for 7 hours, and cool to room temperature Afterwards, the product obtained is suction filtered, the filter cake is repeatedly washed with formic acid and then suction filtered again, and the obtained filter cake is recrystallized with chloroform to obtain zirconocene dichloride;
[0036] (2) Add montmorillonite to distilled water, heat to 70°C and stir for 10 minutes to obtain a montmorillonite solution with a concentration of 1.25...
Embodiment 3
[0042] Indole-3-carbinol was synthesized according to the following steps:
[0043] (1) Add dichloromethane into the reaction flask in the ice-water bath under the protection of nitrogen, start stirring, add zirconium chloride, then add tetrahydrofuran dropwise within 30 minutes, continue stirring for 1 hour, then add diethylamine and cyclopentadiene , the mass ratio of dichloromethane, zirconium chloride, tetrahydrofuran, diethylamine, and cyclopentadiene is 2.47:1.45:3.87:1:1.02, continue stirring for 2 hours, then heat to 45°C for reflux reaction for 7 hours, and cool to room temperature Afterwards, the product obtained is suction filtered, the filter cake is repeatedly washed with formic acid and then suction filtered again, and the obtained filter cake is recrystallized with chloroform to obtain zirconocene dichloride;
[0044] (2) Add montmorillonite to distilled water, heat to 70°C and stir for 10 minutes to obtain a montmorillonite solution with a concentration of 1.25...
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