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关于酮酸合成后处理

作者 Sakura-lin
来源: 小木虫 200 4 举报帖子
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后处理一定要先酸化,碱化再酸化吗?
直接加点盐酸酸化后过柱不行吗?
有大佬合成过吗?求经验分享,谢谢诸位大佬

In a dry, single-neck, 25-mL, round-bottom flask equipped with a stir bar and flushed with nitrogen, the substituted aryl-methylketone (1a–e, 1.0 mmol) and selenium dioxide (SeO2, 0.167 g, 1.5 mmol, 1.5 equiv.) were added followed by anhydrous pyridine (10 mL). The reaction mixture was heated in an oil bath to 110 C for 1 h, and then the bath temperature was reduced to 90 C. The mixture was stirred at this temperature (90 C) for an additional 4 h, and progress of the reaction was monitored by TLC. After completion of the reaction, as determined by TLC, the solution containing precipitated selenium was filtered using a Buckner funnel, and the residue was washed with ethyl acetate (50 mL). The combined filtrate was treated with 1N HCl (20 mL), the organic layer was separated, and the aqueous layer was extracted with ethyl acetate (350 mL). The organic layers were combined and treated with 1N NaOH (50 mL), and the aqueous layer was separated. The organic layer was extracted with water (25 mL) and the combined aqueous layers were acidified using 1N HCl to about pH 1.5. The mixture was extracted with ethyl acetate (350 mL), and the combined organic layers were dried (anhydrous@liuchong630 返回小木虫查看更多

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  • 李ppppN

    酮酸容易脱羧,你要是不怕酮酸分解自然可以酸化之后直接过柱子了,

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