Tris(2,2,2-trifluoroethyl) phosphite

Tris(2,2,2-trifluoroethyl) phosphite was used in the synthesis of N-methoxy-N-methyl bis(2,2,2-trifluoroethyl)phosphonamide via the Arbuzov reaction with 2-bromo-N-methoxy-N-methylacetamide.

Fractionate it through a 10inch Helipak column [Krogh et al. J Org Chem 19 1124 1954]. Tris-[(3-trifluoromethylhydroxymethylene)-d-camphorato] europium (III) [Eu(tfc)3] [34830-11-0] M 893.6, m 195-299o (dec), ~220o, [ ] D +152o (c 2, CCl4, and varies markedly with concentration). Purify it by extraction with pentane, filter and the filtrate is evaporated and the residual bright yellow amorphous powder is dried at 100o/0.1mm for 36hours. A sample purified by fractional molecular distillation at 180-200o/0.004mm gave a liquid which solidified and softened at ~130o, and melted at ~180o and was analytically pure. IR (CCl4) 1630-1680cm-1 and NMR (CCl4) broad: -1.3 to 0.5, -0.08 (s), 0.41 max (s), 1.6-2.3 and 3.39 (s). [McCreary et al. J Am Chem Soc 96 1038 1974, Goering et al. J Am Chem Soc 93 5913 1971.]