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2-BroMo-3',4'-dihydroxyacetophenone synthesis

3synthesis methods
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Yield:40131-99-5 86.3%

Reaction Conditions:

Stage #1: benzene-1,2-diolwith aluminum (III) chloride in dichloromethane at 10 - 15; for 0.5 h;
Stage #2: 2-Bromoacetyl bromide in dichloromethane at -10 - 10; for 10 h;Temperature;

Steps:

1.1 Preparation of 2-bromo-1-(3,4-dihydroxyphenyl)ethanone

1 L of methylene chloride was added to the reaction flask and 276 g of aluminum trichloride was added at 10-15 ° C. After stirring for 20 minutes, 110 g (1. Omol) of catechol was added to the reaction flask in batches, and the stirring was continued for 30 minutes. Then cooled to -10 ° C, and bromoacetyl bromide (202 g (1.0 mol)) was added dropwise. After warming up to 5-10 ° C for 10 hours. After completion of the reaction, 1 L (1.2 mol / L) of dilute hydrochloric acid was quenched at 5-10 ° C, and after the addition of dilute hydrochloric acid, the temperature was stirred at 10 to 15 ° C for 2 hours, and the solid was collected by filtration. The solid was adjusted to about 6.7 with aqueous sodium bicarbonate. After filtration, the solid was collected and dried to give the product 2-bromo-1-(3,4-dihydroxyphenyl)ethanone (199.4 g) in a yield of 86.3%.

References:

CN107011187,2017,A Location in patent:Paragraph 0019