反应 #1785096
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08592470B2
反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mixture of 1,2,4,5-tetrakis-(bromomethyl)-benzene (150 g, 0.33 mmol) and 1,4-dioxane (2 L) was added a 55% aqueous solution of tetrabutylammonium hydroxide (640 mL) at room temperature, followed by stirring at 90° C. for 6 hours. The reaction mixture was allowed to cool to room temperature, and extracted with ethyl acetate after addition of a 2 N aqueous solution of hydrochloric acid (2 L). The organic layer was washed with brine and dried over anhydrous sodium sulfate, and the solvent was distilled away under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9) to give the title compound (35 g, 63% yield). to cool to room temperature extracted with ethyl acetate after addition of a 2 N aqueous solution of hydrochloric acid (2 L) The organic layer was washed with brine dried over anhydrous sodium sulfate the solvent was distilled away under reduced pressure The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9)
来源 ID: ord-ad91ca44d7864a7bbbd3f56b983bcfa8