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ChemicalBook CAS DataBase List 3-CHLOROPHENACYL BROMIDE

3-CHLOROPHENACYL BROMIDE synthesis

5synthesis methods
-

Yield:41011-01-2 91%

Reaction Conditions:

with bromine in n-heptane;water

Steps:

5 EXAMPLE 5
EXAMPLE 5 Under a nitrogen atmosphere, 3'-chloroacetophenone (154.6 g, 1 mol) and anhydrous methanol (310 ml) dried with molecular sieves were charged in a four-necked flask. Bromine (158.2 g, 0.99 mol) was added dropwise with stirring at a temperature in a range from 30° to 45° C. over one hour, and the mixture was maintained at the same temperature for 10 minutes. After water (160 g) was added, the solution was cooled to -10° C. to precipitate crystals which were filtered to obtain 250 g of a crude cake. This crude cake was dissolved in heptane (750 g), and the solution was washed twice with water (200 g), dried over anhydrous magnesium sulfate, filtered, washed and then concentrated to obtain 212.5 g of 2-bromo-3'-chloroacetophenone. The yield was 91.0% and no impurity was detected.

References:

Sumika Fine Chemicals Company, Limited US5717116, 1998, A

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