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ChemicalBook CAS DataBase List 2'-AMINO-4',5'-DIMETHOXYACETOPHENONE
4101-30-8

2'-AMINO-4',5'-DIMETHOXYACETOPHENONE synthesis

7synthesis methods
-

Yield:4101-30-8 94.7%

Reaction Conditions:

with iron;ammonium chloride in water;ethyl acetate at 20; for 4 h;Temperature;Reagent/catalyst;Solvent;

Steps:

2
Compound II 3.40g placed in a 250ml four-necked flask,A mixed solution of ethyl acetate and water (34 ml / 20 ml) was added.At room temperature,To the stirred reaction flask was added 3.55 g of ammonium chloride (0.06644 mol, 4.4 eq).And reduced iron powder 5.92g (0.1057mol, 7eq),The reaction system was then heated to 20 ° C and stirred for 4 h.The progress of the reaction was checked by TLC.After the substrate is completely reacted, the excess iron powder is filtered out.The filter cake was rinsed three times with 15 ml of ethyl acetate.The organic layer was separated from the filtrate and washed with saturated brine.Concentration under reduced pressure gave Compound I 2.79 g, yield: 94.7%, HPLC purity: 99.2%.

References:

Shanghai Pharmaceutical Industry Institute;China Pharmaceutical Industry Zongyuan;Liang Qian;Wang Zhefeng;Yi Bing;Wang Shengli;Zhang Hongliang;Li Changsheng CN108727207, 2018, A Location in patent:Paragraph 0022-0033

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