Method for electrochemically synthesizing key intermediate of tazobactam
A tazobactam, electrochemical technology, applied in the field of electrochemical synthesis of key intermediates of tazobactam, can solve the problems of low selectivity, low reaction efficiency, poor economy, etc., to achieve high selectivity, fast reaction efficiency, The effect of fewer reaction steps
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Embodiment 1
[0039] Example 1: Preparation of 2β-triazolemethyl penicillanic acid diphenylmethyl ester C
[0040]
[0041] At room temperature, a magneton was added to a non-diaphragm electrolytic cell (8 mL), followed by adding disulfide ring opener A (133 mg, 0.25 mmol), 1,2,3-triazole B (138 mg, 2 mmol, 8eq), tetrabutylammonium iodide (185mg, 0.5mmol, 2eq). Acetonitrile (4.5 mL) and acetic acid (0.5 mL) were added using a syringe. After all materials are added, equip with graphite sheet (1×7×0.3cm 3 ) and platinum sheet (1×7×0.3cm 3 ), the electrode immersion area is 2cm 2 (at this time the current density is 4mA / cm 2 ). The reaction solution was stirred for 10 minutes to fully mix, and the DC power supply was adjusted to the constant current mode, and 8mA was electrolyzed at 5F until the raw materials were completely converted. After the reaction, the reaction liquid was sampled and sent to an external standard of HPLC with a yield of 76.8%, and a white solid was obtained thro...
Embodiment 2
[0043] Embodiment 2: Carbon felt is used as anode to prepare 2β-triazole methyl penicillanic acid diphenylmethyl ester C
[0044] At room temperature, a magneton was added to a non-diaphragm electrolytic cell (8 mL), followed by adding disulfide ring opener A (133 mg, 0.25 mmol), 1,2,3-triazole B (138 mg, 2 mmol, 8eq), tetrabutylammonium iodide (185mg, 0.5mmol, 2eq). Acetonitrile (4.5 mL) and acetic acid (0.5 mL) were added using a syringe. After all the materials are added, equip the carbon felt (1×7cm 2 ) and platinum sheet (1×7×0.3cm 3 ) as cathode and anode, electrode immersion area is 2cm 2 . The reaction solution was stirred for 10 minutes to fully mix, and the DC power supply was adjusted to the constant current mode, and 8mA was electrolyzed at 5F until the raw materials were completely converted. After the reaction was finished, the reaction solution was sampled and sent to the HPLC external standard, and the yield was 71.0%.
Embodiment 3
[0045] Embodiment 3: Iron sheet is used as negative electrode to prepare 2β-triazole methyl penicillanic acid diphenylmethyl ester C
[0046] At room temperature, a magneton was added to a non-diaphragm electrolytic cell (8 mL), followed by adding disulfide ring opener A (133 mg, 0.25 mmol), 1,2,3-triazole B (138 mg, 2 mmol, 8eq), tetrabutylammonium iodide (185mg, 0.5mmol, 2eq). Acetonitrile (4.5 mL) and acetic acid (0.5 mL) were added using a syringe. After all the materials are added, equip the graphite sheet (1×7cm 2 ) and iron sheet (1×7×0.2cm 3 ) as cathode and anode, electrode immersion area is 2cm 2 . The reaction solution was stirred for 10 minutes to fully mix, and the DC power supply was adjusted to the constant current mode, and 8mA was electrolyzed at 5F until the raw materials were completely converted. After the reaction, the reaction solution was sampled and sent to the HPLC external standard with a yield of 49.2%.
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