反应 #85070
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06849713B2
反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of potassium phthalimide (8.48 g, 0.046 mol) and 4-bromopropylcyanide (6.4 g, 0.043 mol) in 50 ml of anhydrous DMF was stirred at 90° C. for 2 h. After dilution with 300 ml of water, the aqueous solution was extracted with chloroform (80 ml×3). The combined chloroform solution was washed with 0.5% NaOH aqueous solution (80 ml) and water (100 ml), and dried over anhydrous Na2SO4. After evaporation of chloroform, an oil was obtained and 300 ml of water was added. The oil was rapidly solidified. The solid formed was collected by filtration, washed with water, and dried under high vacuum. The product was recrystallized from methanol which was diluted with water, to give white crystals (7.75 g, 84%). 1H NMR (CDCl3) δ7.87 (dd, 2H), 7.75 (dd, 2H), 3.83 (t, 2H), 2.44 (t, 2H), 2.09 (quintet, 2H). After dilution with 300 ml of water, the aqueous solution was extracted with chloroform (80 ml×3) The combined chloroform solution was washed with 0.5% NaOH aqueous solution (80 ml) and water (100 ml) dried over anhydrous Na2SO4 After evaporation of chloroform an oil was obtained The solid formed was collected by filtration washed with water dried under high vacuum The product was recrystallized from methanol which was diluted with water
来源 ID: ord-d989185980c245c7bc26ebeea978d823