ETHYL ACETOACETATE PROPYLENE GLYCOL KETAL synthesis

Yield:6290-17-1 98%

Reaction Conditions:

with Amberlyst₁₅ in cyclohexaneReflux;

Steps:

2 Example 2
Ethyl acetoacetate (0.1mol), cyclohexane (50mL), 1,2-propanediol (0.15mol) were added to a 250mL three-necked round bottom flask containing 2g of catalyst Amberlyst15, a magnet and a thermometer were added, and water was added. The temperature was raised to reflux, and the reaction was monitored by GC. When the reaction is complete, filter the catalyst. Among them, the catalyst is recovered and washed with acetone, and baked at 80°C for one hour to recover the catalyst; the liquid phase is washed with saturated sodium bicarbonate solution and separated, the organic phase is separated and washed with saturated brine, and then distilled under reduced pressure to obtain ethyl acetoacetate ester.According to gas chromatography (GC) analysis, the yield of the catalyzed fructone in this example reached 98percent, and the selectivity was 99.0percent.

References:

Shenzhen Qian Haiboyang Institute Co., Ltd.;Xiong Donglu;Xu Tao;Long Xujian;Xiao Zengjun;Yi Song;Yang Xuan CN111333607, 2020, A Location in patent:Paragraph 0039-0041

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