關(guān)于酮酸合成后處理
后處理一定要先酸化,堿化再酸化嗎?
直接加點鹽酸酸化后過柱不行嗎?
有大佬合成過嗎?求經(jīng)驗分享,謝謝諸位大佬
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
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酮酸容易脫羧,你要是不怕酮酸分解自然可以酸化之后直接過柱子了,