Twenty nine bis (fluoroalkyl) phosphates (RFO) 2P (O) OR were prepared in 18–75% yield by treating phosphorochloridates (RFO) 2P (O) Cl, where RF was HCF2CH2, HCF2CF2CH2, H (CF2) 4CH2, C2F5CH2, C3F7CH2,(CF3) 2CH,(FCH2) 2CH and (CH3) 2CF3C with methanol, ethanol, propanol and isopropanol in diethyl ether in the presence of triethylamine. The bulky chloridate [(CH3) 2CF3CO] 2P (O) Cl reacted with methanol, ...