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ChemicalBook CAS DataBase List Dimethyl 2,2'-azobis(2-methylpropionate)

Dimethyl 2,2'-azobis(2-methylpropionate) synthesis

5synthesis methods
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Yield:2589-57-3 94.9%

Reaction Conditions:

with thionyl chloride in 1,2-dichloro-ethane at 15 - 32; for 6 h;Temperature;Solvent;Reagent/catalyst;

Steps:

1-5 Example 5
In a 500 ml three-necked flask with a stirring and reflux device,41.8 g of 98% 2,2’-azobisisobutyronitrile (0.25 mol) and 200 g of dichloroethanePut 33.6 g of 99.9% methanol (1.05 mol), start stirring,Start cooling to 15 deg.] C was slowly added dropwise 66.1 g of 99% thionyl chloride (0.55mol),The dropping rate of sulfoxide was 16 g / hour.Then the temperature of the material was controlled at 32 ° C, and the temperature was maintained for 6 hours.After the reaction was completed, 104.5 g of cold water at 7 ° C was added dropwise to carry out the hydrolysis reaction.After 1 hour of reaction, the layers were separated. The organic phase is washed with an appropriate amount of water and separated into layers.The organic phase is distilled under reduced pressure until all dichloroethane is recovered by distillation.This gave liquid dimethyl azobisisobutyrate. Dimethyl azobis isobutyrate liquid cryogenic cooling to obtain a white solid product dimethyl azobis isobutyrate.The yield (based on 2,2'-azobisisobutyronitrile) was 94.9%. Product content (HPLC) 99.8%.

References:

Shanghai Shi Si Hewei Chemical Co., Ltd.;Liang Junlong;Liu Jialei CN110256281, 2019, A Location in patent:Paragraph 0008; 0021-0038

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