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1-(3-amino-5-bromo-2-hydroxyphenyl)ethanone synthesis

4synthesis methods
Preparation by reaction of 20% aqueous titanium trichloride solution on 5-bromo-2-hydroxy-3-nitroacetophenone in toluene, at r.t., in a sealed tube (31%).
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Yield:70977-85-4 83%

Reaction Conditions:

with hydrogenchloride;zinc(II) chloride in acetonitrile at 50; for 20 h;Large scale;

Steps:

1.3 Step 3: Preparation of 2-hydroxy-3-amino-5-bromoacetophenone

Acetylamino-4-bromophenol 114kg, dissolved in 200kg of acetonitrile,10 kg of ZnCl2 was added and the temperature was raised to 50 ° C. A dry hydrogen chloride gas was introduced into the reaction system,Reaction for 20 h, after the end of the reaction, the recovery of most of the solvent,To the system by adding 200kg 2Mol / L dilute hydrochloric acid,Heating reaction reflux 4h, after the end of the reaction, the reaction system cooled to room temperature,6 mol / L sodium hydroxide solution was added to the reaction system to pH to 9-10. The solid was precipitated, filtered, washed with water and dried to give 95 kg of a pale yellow solid in 83% yield.

References:

CN107098822,2017,A Location in patent:Paragraph 0017