Synthesis method of diisopropyl azodiformate
A technology of diisopropyl azodicarboxylate and diisopropyl hydrazine dicarboxylate, which is applied in the field of organic chemical synthesis, can solve the problems of serious environmental pollution, large discharge of three wastes, large energy consumption, etc., and achieve high product purity , The effect of low oxidant cost and low energy consumption
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Embodiment 1
[0015] In a 500ml three-necked flask equipped with a thermometer, dropping funnel and agitator, add 10g of diisopropyl hydrazine dicarboxylate and 100ml of water, add 20ml of 50% concentrated sulfuric acid while stirring, and then add 0.05g of 40% hydrobromic acid 13g of 10% hydrogen peroxide was added dropwise at -15°C, the dropwise addition was completed in 0.5h, then stirred for 1h, left standing after the reaction was completed, the oil phase was separated, and the 2 Cl 2 Extract the water phase, combine the oil phase with the extract, wash with water until neutral, and wash with anhydrous MgSO 4 After drying and distilling off the solvent, 9.4 g of diisopropyl azodicarboxylate (93% yield, 99.5% purity) was obtained, and its H NMR and IR spectra were consistent with those of the standard sample.
Embodiment 2
[0017] In a 500ml three-necked flask equipped with a thermometer, a dropping funnel, and a stirrer, add 10g of diisopropyl hydrazine dicarboxylate, 100ml of water, add 20ml of 40% sulfuric acid under stirring, and then add 0.05g of 40% hydrobromic acid, Add 13g of 10% hydrogen peroxide dropwise at 0°C for 0.5h, then stir for 6h, let stand after the reaction is complete, separate the oil phase, and use CH 2 Cl 2 Extract the water phase, combine the oil phase with the extract, wash with water until neutral, and wash with anhydrous MgSO 4 After drying and distilling off the solvent, 9.6 g of diisopropyl azodicarboxylate (95% yield, 99.4% purity) was obtained, and its H NMR and IR spectra were consistent with those of the standard sample.
Embodiment 3
[0019] In a 500ml three-necked flask equipped with a thermometer, a dropping funnel, and a stirrer, add 10g of diisopropyl hydrazine dicarboxylate, 100ml of water, add 20ml of 30% sulfuric acid under stirring, and then add 0.2g of 40% hydrobromic acid, Add 13g of 10% hydrogen peroxide dropwise at 0°C for 0.5h, then stir for 6h, let stand after the reaction is complete, separate the oil phase, and use CH 2 Cl 2 Extract the water phase, combine the oil phase with the extract, wash with water until neutral, and wash with anhydrous MgSO 4 After drying and distilling off the solvent, 9.6 g of diisopropyl azodicarboxylate (95% yield, 99.5% purity) was obtained, and its H NMR and IR spectra were consistent with those of the standard sample.
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