Preparation of Laurie Diethanolamide from Lauroyl Chloride

Preparation of Laurie Diethanolamide from Lauroyl Chloride 

Part A.— About 202 grams (1 mol) of melted lauric acid (90%) was mixed with about 35 mL. (0.4 mol) of phosphorus trichloride at a temperature of approximately 40° C. After the resultant mixture had separated into two immiscible liquid layers, the lower layer consisting essentially of phosphorous acid was separated from the lauroyl chloride present in the upper layer. 

Part C.—The upper organic layer was removed and diluted with about 100 mL. of chlorinated solvent and azeotropically distilled until substantially all water had been removed. The cooled anhydrous solution was then filtered to remove precipitated salts and soaps after which the clear filtrate was distilled, the last traces of solvent being removed under reduced pressures, e. g., about 10 mm. mercury and at a temperature not exceeding 100° C. The pale liquid residue crystallized to a low-melting waxy material containing about 96% lauric diethanolamide, about 3% lauric acid, and about 1% diethanolamine ester. Source Krems 1954 

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