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ChemicalBook CAS DataBase List 3,4-Methylenedioxyacetophenone
3162-29-6

3,4-Methylenedioxyacetophenone synthesis

8synthesis methods
3,4-Methylenedioxyacetophenone's synthesis method: 1) from Piperonylic acid plus Acetic acid vapors at high temperature over catalyst (Thoria, e.g.). 2) from alpha-Methylpiperonylic acid by oxidation.
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Yield:3162-29-6 96%

Reaction Conditions:

in nitrobenzene at 80;Friedel-Crafts Acylation;

Steps:

3 Embodiment 3
In a 1 L three-opening in the bottle, to join the nitrobenzene 500 ml, aluminum chloride/silicon dioxide (166.3 g, loading 10 wt %), stirring slowly into the acetic acid under the condition (33.0 g, 0 . 55 μM), the completion of the dropping, then gradually dripped into the pepper link (61.0 g, 0.5 μM, dissolved in 100 ml of nitrobenzene); after dropping, slow heating to 80 °C stirring reaction, until the pepper ring reaction finishes, cooling, filtering to obtain aluminum chloride/silicon dioxide catalyst; the reaction liquid layered extraction, the combined organic layer, evaporating the solvent under reduced pressure, drying to obtain products 78.8 g, yield 96%.

References:

Zhejiang Xinhecheng Co., Ltd.;Zhou Yougui;Hu Boyan;Yu Ming;Zhang Yuhong;Li Qichuan CN107434798, 2017, A Location in patent:Paragraph 0035-0042

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