In this study, perthiophosphonic acid anhydrides which are previously known (2,4-bis(3-methoxytolyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide ([(3-methoxytolyl)P(S)S)2], SAV-B1 reagent and 2,4-bis(ferrocenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide [(ferrocenyl)P(S)S)2], FcLR, Ferrocenyl Lawesson's Reagent) react with alcohols to obtain new dithiophosphonic acids (3-methoxytolyl=(CH3)(OCH3)C6H3- and Xn=alkyl group (R) for SAV-B1, HXn; R1=3-pentyl-, HX1; R2=2-butyl-, HX2; R3=2-pentyl-, HX3 and Fc=Ferrocenyl- and Yn=allkyl or aryl group (R’) for FcLR, HYn; R’1=4-tert-cyclohexyl-, HY1; R’2=2-phenyl-1-propyl-, HY2). These acids were then converted to ammonium salts ([NH4][Xn], [NH4][Yn]). The structures of ammonium salts were characterized by mass-(ESI), FT-IR, 1H-, 13C- and 31P-NMR spectroscopy and elemental analysis.