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ChemicalBook CAS DataBase List 2',3',4'-TRIHYDROXYACETOPHENONE
528-21-2

2',3',4'-TRIHYDROXYACETOPHENONE synthesis

11synthesis methods
Preparation by Fries rearrangement of pyrogallol triacetate with aluminium chloride without solvent.
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Yield:528-21-2 173.45 g

Reaction Conditions:

with glacial acetic acid;stannous chloride at 35; for 12 h;

Steps:

1 Example 1: Preparation of Compound 1

Add acetic acid (1000mL) and pyrogallol (200g, 1.59mol) to the reaction flask, stir, add anhydrous tin chloride (98.26g, 0.48mol), slowly add acetyl chloride (136.94g, 1.74mol) dropwise, The temperature was controlled below 35°C, and after the dropwise addition, the stirring reaction was continued for 12 hours. The reaction solution was cooled to 0°C, ice water (1000mL) was added dropwise, the temperature was controlled below 10°C, after the dropwise addition, the mixture was stirred at 0°C for 1 hour, filtered, and the filter cake was washed with ice water (500mL). Drying under reduced pressure at 50°C gave 173.45 g of compound 1 as a dark yellow solid.

References:

CN114276321,2022,A Location in patent:Paragraph 0006; 0017-0018

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