Electrochemical preparation method of ozanimod intermediate
An intermediate and electrode technology, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large environmental pollution and large amount of inorganic reducing agent zinc powder, so as to simplify the process flow and reduce the production cost. Effect
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Embodiment 1
[0052] Electroreduction Preparation of 1-amino-4-cyano-2,3-dihydroindene
[0053]
[0054] Install split electrolyzer, N-117 proton membrane. Add 0.34g (1.98mmol) 4-cyanoindanone oxime to the cathode chamber, dissolve the substrate with 7mL acetonitrile, add 38mL 0.5mol / L Na 2 HPO 4 The solution was used as the electrolyte; 45 mL of 1.5 mol / L NaOH solution was added to the anode compartment as the electrolyte. The cathode electrode is a lead sheet (2×2cm 2 ), the anode electrode is a platinum sheet (1×1cm 2 ), the cell voltage is 5.0V, the current is 26mA, the working potential is about 1.6V, the constant temperature is 40°C, and the electrolysis is 17h. Take the catholyte and remove acetonitrile by rotary evaporation, extract the remaining alkaline aqueous solution twice with ethyl acetate, adjust the pH=8 to 9 with dilute hydrochloric acid solution, extract once more, combine the extracts, Na 2 SO 4 Drying and precipitation, the yellow-green oily compound was obtain...
Embodiment 2
[0056] Electroreduction Preparation of 1-amino-4-cyano-2,3-dihydroindane
[0057]
[0058] Install split electrolyzer, N-117 proton membrane. Cathode (zinc sheet, 2×2cm 2 ) room, add 0.34g (1.98mmol) 4-cyano 2,3-indanone oxime, dissolve the substrate with 7mL acetonitrile, add 38mL 0.5mol / L Na 2 HPO 4 solution as electrolyte; anode (platinum mesh, 1×1cm 2 ) chamber, add 45mL of 1.5mol / L NaOH solution as electrolyte. The tank voltage is 5.0V, the current is 26mA, the working potential is about 1.6V, the constant temperature is 40°C, and the electrolysis is 17h. Take the catholyte and remove acetonitrile by rotary evaporation, extract the remaining alkaline aqueous solution twice with ethyl acetate, adjust the pH=8 to 9 with dilute hydrochloric acid solution, extract once more, combine the extracts, Na 2 SO 4 Drying and precipitation, the yellow-green oily compound was obtained. Add 3mL of tetrahydrofuran, inject HCl gas, and a white solid (1-amino-4-cyano-2,3-dihydroin...
Embodiment 3
[0060] Electroreduction Preparation of 1-amino-4-cyano-2,3-dihydroindane
[0061]
[0062] Install split electrolyzer, N-117 proton membrane. Cathode (zinc sheet, 2×2cm 2 ) room, add 0.34g (1.98mmol) 4-cyano 2,3-indanone oxime, dissolve the substrate with 7mL acetonitrile, add 38mL 0.5mol / L Na 2 HPO 4 solution as electrolyte; anode (platinum mesh, 1×1cm 2 ) chamber, add 45mL of 1.5mol / L NaOH solution as electrolyte. The tank voltage is 5.0V, the current is 26mA, the working potential is about 1.6V, the constant temperature is 30°C, and the electrolysis is 17h. Take the catholyte and remove acetonitrile by rotary evaporation, extract the remaining alkaline aqueous solution twice with ethyl acetate, adjust the pH=8 to 9 with dilute hydrochloric acid solution, extract once more, combine the extracts, Na 2 SO 4 Drying and precipitation, the yellow-green oily compound was obtained. Add 3mL of tetrahydrofuran, inject HCl gas, and a white solid (1-amino-4-cyano-2,3-dihydroin...
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