Organic compounds -- part of the class 532-570 series – Organic compounds – Phosphorus containing
Patent
1997-11-12
1999-04-06
Geist, Gary
Organic compounds -- part of the class 532-570 series
Organic compounds
Phosphorus containing
C07F 953
Patent
active
058921214
ABSTRACT:
A process for the purification of tertiary phosphine oxides obtained in a Wittig synthesis as a contaminated by product resulting from the reaction of the corresponding tertiary phosphines, especially triphenylphosphine. The contaminated tertiary phosphine oxides coming from this Wittig synthesis have the formula I ##STR1## in which R.sup.1, R.sup.2, and R.sup.3 denote C.sub.1 -C.sub.12 alkyl, C.sub.5 -G.sub.8 cycloalkyl, aryl, C.sub.7 -C.sub.20 aralkyl, or C.sub.7 -C.sub.20 alkylaryl. The contaminated phosphine oxide I or phosphine oxide I-containing mixtures, optionally in an inert solvent, are first caused to react with an inorganic or organic acid at temperatures of from 0.degree. to 150.degree. C. to form a crystallized acid salt. The resulting salt crystals are then treated in a purifying step with water or an inorganic base or an organic base to again form the tertiary phosphine oxide. This reformed oxide is then extracted with an inert organic solvent from which the purified tertiary phosphine oxide is finally liberated.
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Hermeling Dieter
Hugo Randolf
Siegel Hardo
BASF - Aktiengesellschaft
Geist Gary
Padmanabhan Sreeni
Shurtleff John H.
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