Electric Literature of 16355-92-3, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 16355-92-3 as follows.
First, 260.3 g (2.0 mol) of ethyl acetoacetate and 500 ml of acetone were fed into a 2 L four-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and after stirring and mixing, 97 mass 61.9 g (1.5 mol) of% sodium hydroxide was added and allowed to react for 15 minutes. Next, after adding 197.0 g (0.5 mol) of 1,10-diiododecane, the mixture was refluxed.For 6 hours.[0139]After completion of the reaction, acetone was removed by distillation under reduced pressure, and 2N hydrochloric acid was added to neutralize, followed by liquid separation treatment.The upper organic layer was separated from the lower water tank. After the separation treatment, the upper organic layer and 800 g of a 10% by mass aqueous sodium hydroxide solution (2.0 mol)And saponification reaction at room temperature for 8 hours, and then 50% by weight sulfuric acid aqueous solution 205.8 g (1.1 mol) was added and the whole was refluxed for 3 hours to carry out a decarboxylation reaction. After completion of the decarboxylation reaction, the upper organic layer (dissolved 2,15-hexadecanedione) is obtained by liquid separationAnd the sulfuric acid layer are separated, and the organic layer is cooled to room temperature to give 2,15-hexa130.8 g of a crude product of decanedione was obtained. A part of the obtained crystal was collected and analyzed by gas chromatography.The conversion of iododecane is 100%, the purity of 2,15-hexadecanedione is 92%,The yield of 2,15-hexadecanedione based on 10-diiododecane was 95%.
According to the analysis of related databases, 16355-92-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Toho Earth Tech Co., Ltd.; Kazama, Shoutarou; toishi, Shoushi; Takizawa, Kazuhiro; (21 pag.)JP6572399; (2019); B1;,
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