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ChemicalBook CAS DataBase List N-LAURYLDIETHANOLAMINE
1541-67-9

N-LAURYLDIETHANOLAMINE synthesis

6synthesis methods
-

Yield:1541-67-9 98%

Reaction Conditions:

with potassium carbonate;potassium iodide in acetonitrile for 12 h;Inert atmosphere;Reflux;

Steps:

5
1) dibasic bromide (7.48 g, 30 mmol), diethanolamine (4.73 g, 45 mmol)Anhydrous potassium carbonate (8.29 g, 60 mmol) and potassium iodide (1.0 g) were added to a 250 mL two-necked flask, 80 mL of acetonitrile was added, and the mixture was bubbled with nitrogen for 5 minutes.Air, then reflow 12h.(029) (2) To stop the reaction, acetonitrile was removed by steaming, 60 mL of dichloromethane and 60 mL of water were added thereto, and the mixture was separated. The organic phase is washed with waterTimes to remove excess diethanolamine. Product in the water have a certain solubility, washed, the water phase and then dichloromethaneExtraction twice. The organic phase was separated and dried over anhydrous sodium sulfate.[0060] (3) Removal of methylene chloride by steam to give 8.04 g of pale yellow liquid, 98.0% yield JLC test, ethyl acetate / petroleumEther = 1: 1 as the developing agent, the target product than the shift value Rf = 0.35.(3) The procedure of step (3) was carried out in a 250 mL single-necked flask to prepare 8.0 g (30 mmol) of dodecyldiethanolamine, 4.64 g (39 mmol) of bromopropyne and 100 g of ethanol, and the mixture was stirred and refluxed for 12 h with stirring.(5) The excess bromine propyne and solvent ethanol were distilled off under reduced pressure to give 11.75 g of the crude product as brownish red viscous liquid,99.0HC detection, dichloromethane: methanol = 6: 1, the ratio of the value of Rf = 0.50.(6) dichloromethane: methanol = 10: 1, silica gel column chromatography to obtain pure product C12 as a white waxy solid.

References:

China University of Petroleum,Beijing;LIU, Dong-dong;YAO, Erdong;ZHOU, Fu-jian;YAN, Wei;SONG, Yan;JIANG, Zhenxue;GAO, zhi ye;LI, Zhuo;YANG, Wei;LIU, Che;LI, Yuan CN106187790, 2016, A Location in patent:Paragraph 0057-0063

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