105-53-3, A common compound: 105-53-3, name is Diethyl malonate, belongs to esters-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.
Diethyl malonate (20 g, 0.125 mol), triethylamine (25.3 g, 0.25 mol), magnesium chloride (11.9 g, 0.125 mol), acetonitrile (200 ml) were placed in a reaction flask, and the temperature was lowered to -5. C, slowly add acetyl chloride (10g, 0.125mol), temperature control -5C, about 30min drop, after lh incubation, rose to room temperature for 8h. After TLC monitoring reaction, adjust the pH to about 3 with 1N HCl, extract twice with ether, combine the organic phase, wash with 1N HCl, no Dry with sodium sulfate, evaporated to dryness, and the residue was dissolved with DMF.Add bromoethane (16.2 g, 0.148 mol), potassium carbonate (21 g, 0.149 mol), potassium iodide (2.1 g, 0.012 mol), and react at 60 C for 2 h. After the reaction was completed by TLC, the reaction mixture was cooled to room temperature and water was added. , ether, stirring, layering,The organic layer was washed with saturated brine.Dry and evaporate to give a yellow oil, 22 g.Purification by column chromatography gave 7.4 g of pale yellow oil.Yield: 25.8 %.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Diethyl malonate, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Shenyang Hainuowei Pharmaceutical Technology Co., Ltd.; Wang Shaojie; Mao Qing; Zhang Bing; (30 pag.)CN110156698; (2019); A;,
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