Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 100-37-8, name is 2-(Diethylamino)ethanol. A new synthetic method of this compound is introduced below., Application In Synthesis of 2-(Diethylamino)ethanol
165 g of ibuprofen and 160 mL of isopropyl acetate were placed in a pre-dried 500 mL three-necked flask and equipped with a reflux and agitation device; 64 mL of thionyl chloride was slowly added to the three-necked flask with stirring, and the mixture was stirred at room temperature for 30 minutes and then heated to reflux. Keep refluxed for 2-3 hours; The reaction mixture was rotary evaporated until No fraction dropout, and evaporated to dryness by adding 120 mL of n-hexane, and 120 mL of isopropyl acetate was added thereto, and the distillation was continued until no fraction was dropped, and the distillation was repeated once with isopropyl acetate. The evaporated mixture was dissolved in 600 mL of isopropyl acetate and transferred to a pre-dried 2 L three-necked flask, stirred and cooled to below 10 C; 93.6g of 2-(diethylamino)ethanol was slowly added dropwise to the above three necked flask through a constant pressure dropping funnel, and the temperature was controlled within 10 C, after the completion of the dropwise addition, stirring was continued at 0-10 C for 0.5 hours; 88 g of anhydrous potassium carbonate solid was added to the above three-necked bottle in portions, stirred at 5-10 C for 30 minutes, then slowly warmed to 15-25 C, and stirred at this temperature for 8-10 hours; 320 mL of deionized water was added to the above reaction solution, stirred for 15-30 minutes, and the organic phase was separated. The organic phase was washed four times with deionized water (320 mL X 4) and dried over anhydrous sodium sulfate. Filtration, then washed solid sodium sulfate with a small amount of isopropyl acetate; The above organic phase was transferred to a 2L three-necked flask, and the temperature was lowered to below 10 C, and about 32 g of hydrogen chloride gas was introduced at 0-10 C and maintained it for 1- 2 hours, then Concentrated a part of the solution, added 120 mL of n-hexane under stirring, added 1 g of seed crystals, and sealed and placed in refrigerator for crystallization; Filtration, washing with ethyl acetate / n-hexane (V / V = 1:1, 200 ml X 2); The obtained solid was dried under vacuum at 40-50 C until the water (moisture content )is qualified, to obtain 178.56 g of a crystalline crystal, a molar yield of 65.2%, and a purity of 99.76 %.
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Reference:
Patent; Tianjin Xinchen Taifeier Pharmaceutical Technology Co., Ltd.; Yao Chen; (25 pag.)CN108727206; (2018); A;,
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