Rapid and Efficient Synthesis of -Alkylenediphosphoric Acids from Phosphorus Oxychloride

Table 1

Reaction conditions and results of the synthesized products with the different methods.

	Yield (%)
Diols
Method 1; °C, , –10 h,; solvent: toluene	70	65	85
Method 2; °C → 20°C, , ,  h,; solvents: THF () or diethyl ether ( and )	65	62	75
Method 3; °C, ,  min,; W, solvent: acetonitrile	65	68	72

: reaction time (step 1), : molar ratio POCl₃/diol, : molar ratio triethylamine/diol, : hexane-1,6-diol, : nonane-1,9-diol, and : dodecane-1,12-diol.
Products were not obtained in pure form (maximum purity a: 95%, b: 90%).