反应 #3191695
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07595397B2
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2 g of 3-isopropyl-piperazine-2,5-dione could be suspended in anhydrous THF under nitrogen and cooled in an ice-bath. 4 equiv. of lithium aluminium hydride could be added. The reaction could be stirred at 0° C. for 0.5 h, then heated to reflux overnight. The reaction could be quenched by the subsequent addition of 1 mL/gLiAlH4 of water, 1 mL/gLiAlH4 of 5% aqueous sodium hydroxide solution and 3 mL/gLiAlH4 of water. The resulting solid could be separated by filtration through Celite and rinsed with ethyl acetate. The filtrate could be concentrated in vacuo to afford 2-isopropyl-piperazine. cooled in an ice-bath The reaction heated to reflux overnight The reaction could be quenched by the subsequent addition of 1 mL/gLiAlH4 of water, 1 mL/gLiAlH4 of 5% aqueous sodium hydroxide solution and 3 mL/gLiAlH4 of water The resulting solid could be separated by filtration through Celite rinsed with ethyl acetate The filtrate could be concentrated in vacuo
来源 ID: ord-317ed03dc2f9415daf9faf2d8f81eaab