反应 #98525
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05416065
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 41.8 g of hydrazine-N,N'-dicarboxylic acid di-tert-butyl ester, 74.5 g of potassium carbonate, 52.0 g of 2,2-dimethyl-1,3-propanediol dimethanesulfonate and 2.0 g of potassium iodide are stirred for 48 hours at 120°-130° C. in 360 ml of N,N-dimethylformamide. The reaction mixture is then concentrated; diethyl ether is added and the organic phase is washed with water. Mter drying over sodium sulfate, the reaction mixture is concentrated and purified by means of column chromatography to yield 1.1 g of the desired product, 4,4-dimethyl-pyrazolidine-N,N'-dicarboxylic acid di-tert-butyl ester, in the form of white crystals. The reaction mixture is then concentrated diethyl ether is added the organic phase is washed with water Mter drying over sodium sulfate the reaction mixture is concentrated purified by means of column chromatography
来源 ID: ord-d11c6c925c1348ed84d5539cdd66929d