The present invention is concerned with an improved process for the preparation of alkylphosphocholines and anti-leishmanial drug Miltefosine. Commercially available, 2-chloro-1,3,2-dioxaphospholane (CAS: 822-39-9) is the key starting material which upon treating with n-alkanols in an inert solvent in the presence of a base in a single vessel and subsequent reaction of the resulting intermediate with a halogen followed by evaporation and treating the residue in the same vessel with aqueous trimethylamine afforded alkylphosphocholines. Purification by reverse-phase flash column chromatography afforded alkylphosphocholines in an overall good yield without isolation of any intermediates. Most importantly, the process is expedient and improved compared to the earlier methods of producing alkylphosphocholines and Miltefosine thereof in pure form.