反应 #1822734
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05187286
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 25 g of trans-4-cyclohexene-1,2-dicarboxylic acid diethyl ester in 140 ml of tetrahydrofuran is instilled in a suspension of 10 g of lithium aluminum hydride in 140 ml of tetrahydrofuran at room temperature and the mixture is then stirred for 3 hours at reflux temperature. It is cooled to 0° C., a mixture of tetrahydrofuran/water (1+1) is instilled slowly, stirred for 30 minutes, mixed with 150 ml of chloroform, filtered and the filtrate is concentrated by evaporation in a vacuum. The residue is distilled at 0.2 mm/Hg and at 150° C. in a bulb tube. In this way, 20 g of trans-1,6-dihydroxymethyl-3-cyclohexene is obtained as a colorless oil. at reflux temperature stirred for 30 minutes filtered the filtrate is concentrated by evaporation in a vacuum The residue is distilled at 0.2 mm/Hg and at 150° C. in a bulb tube
来源 ID: ord-fe329a9fd14842c0b7192036058f5c2d