A general method for the separation of triphenylphosphine oxide and reaction products using high performance countercurrent chromatography

作者：Edwards Neil A^*; Fisher Gail; Harris Guy H; Kellichan Nikki

来源：Journal of Chromatography A, 2014, 1323: 49-56.

DOI：10.1016/j.chroma.2013.10.089

• Countercurrent chromatography
• Preparative chromatography
• Reverse phase liquid chromatography
• Triphenylphosphine oxide
• Impurity removal
• Mitsunobu reaction

A standardised separation methodology was developed for the purification of crude reaction mixtures containing triphenylphosphine oxide (TPPO) using high performance countercurrent chromatography (HPCCC). A solvent system consisting of hexane/ethyl acetate/methanol/water (5:6:5:6) was used in 1 column volume elution extrusion mode. The HPCCC methodology was compared with classical RP HPLC purification using a set of 12 representative Mitsunobu reaction mixtures. HPCCC was seen to yield a 65% increase in the average recovery of the target component whilst providing similar final target purities to those obtained by HPLC. By eliminating the need for method development for individual samples, the HPCCC methodology described within provides a simple and efficient means for the purification of the entire family of TPPO-containing reaction products.

• 出版日期2014-1-3