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ChemicalBook CAS DataBase List 1-Bromoethyl acetate

1-Bromoethyl acetate synthesis

4synthesis methods
1-bromoethyl acetate is prepared by reacting acetyl bromide and acetaldehyde using zinc chloride as a catalyst. 
After cooling 30 ml of hydrogen bromide / acetic acid (1.2 equiv) to 0 ° C., 53.5 ml (1.0 equiv) of vinyl acetate was slowly added thereto, followed by stirring for 1 hour. It was extracted with dichloromethane, washed with distilled water at 0-5 ° C., dehydrated with anhydrous magnesium sulfate, and distilled under reduced pressure to obtain 81.4 g of 1-bromoethyl acetate.
synthesis of 1-bromoethyl acetate
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Yield:40258-78-4 89%

Reaction Conditions:

with iron(III) oxide;tetrabromosilane in water at 12 - 20; for 0.5 h;Temperature;

Steps:

6
42.0 mL of pure water and 0.312 g of nanometer ferroferric oxide were added to the reaction flask equipped with a mechanical stirrer, and the temperature was maintained at 12 ° C.After stirring for 5 min, 120 mL of silicon tetrabromide was added, and after stirring for 10 min, 312 mL of vinyl acetate was slowly added, and the temperature was adjusted to 20 ° C.The reaction was terminated in 30 min;The nanometer ferroferric oxide was separated from the mixed solution by a magnet, and the mixture was passed through a 0.22 μm organic filter to remove solid impurities; the mixture was cooled to 2 ° C and maintained.78 mL of extractant was added thereto, stirred for 10 min, then 45 mL of pure water was added, stirred for 10 min, allowed to stand for 10 min, the organic phase was taken, 25 mL of pure water was added and stirred for 5 min, allowed to stand for 5 min, and the organic phase was distilled under reduced pressure to remove the fraction.That is, the product 1-bromoethyl acetate.The extractant is a mixture of dichloromethane and chloroform in a volume ratio of 2:1.The yield was 89.0% and the purity was 98.2%.

References:

Guangdong Liguo Pharmaceutical Co., Ltd.;Zeng Jianjiang;Wang Bao;Xu Weilong;Liao Qingfan;Wang Xiongqiang;Chen Kaiming CN108383727, 2018, A Location in patent:Paragraph 0052-0053; 0056-0057; 0061-0062; 0065-0074

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