A convenient method for the preparation of phosphatidylcholines is proposed, which is based upon phosphorylation of diglycerides with phosphorus oxychloride followed by a reaction of the resulting dichlorophosphates with choline tetraphenylborates. This requires no isolation of intermediates and affords phosphatidylcholines with >60% yields. By its use, two novel ester and ether phosphatidylcholines with deuterium labels in the hydrophilic moiety, rac-1,2-dihexadecylglycero-3-phospho(H-2(13))choline and rac-1,2-dipalmitoylglycero-3-phospho(H-2(13))choline, were synthesized.