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ChemicalBook CAS DataBase List 2-Bromomethyl-1,3-dioxolane
4360-63-8

2-Bromomethyl-1,3-dioxolane synthesis

9synthesis methods
Ethylene glycol

107-21-1

Acetaldehyde

75-07-0

2-Bromomethyl-1,3-dioxolane

4360-63-8

10.326 kg (166.3 mol) of ethylene glycol and 3.66 kg (83.185 mol) of freshly distilled acetaldehyde were added to the reaction vessel with slow stirring at room temperature for 30 minutes. Slowly 14.622 kg (91.504 mol) of bromine was added dropwise, with the rate of dropwise acceleration being controlled to maintain the reaction temperature at 0-3 °C. After the dropwise addition was completed, the reaction was continued at 0-3 °C for 3.5 hours. Upon completion of the reaction, decompression distillation was carried out to collect the fraction at 80-82 °C/3.6 kPa to give 11.002 kg (65.883 mol) of 2-bromomethyl-1,3-dioxolane in 79.2% yield, which was analyzed to be greater than 95%.

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Yield:4360-63-8 79.2%

Reaction Conditions:

Stage #1:ethylene glycol;acetaldehyde at 20; for 0.5 h;Large scale;
Stage #2: with bromine at 0 - 3; for 3.5 h;Large scale;Temperature;

Steps:

1.b b. Preparation of bromoacetaldehyde ethylene glycol
To a reaction vessel, 10.326kg (166.3mol) of ethylene glycol was added with 3.66 Kg (83.185mol) of freshly distilled acetaldehyde and stirred slowly at room temperature for 30 mins. 14.622 Kg (91.504 mol) of bromine was added dropwise, after the dropwise addition, the reaction was carried out at 0-3°C for 3.5h, and the fraction was distilled under reduced pressure. The fractions (3.6 kPa) and 11.002 Kg (65.883 mol) of 80-82 ° C were collected and identified as bromoacetaldehyde ethylene glycol, the yield is 79.2%, the content is more than 95%.

References:

Beijing Yifang Biological Technology Co., Ltd.;Wang, Jiao;Shi, Qingdong CN105418612, 2016, A Location in patent:Paragraph 0028; 0039; 0040

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