preparation of Methyl triphenyl Phosphonium Acetate

the correspongind phosphonium bromide 1 eq.
dissolve in DCM. (0.5 M)
NaOH 2 eq. dissolve in water. 1 M.
then put the two solutions together in a separatory funnel, shake vigorously for 10 min at rt.
then organic layer separated. washed with nahco3, brine.
concentrated to 50 ml or until solid started to showup.
then hexanes 100 ml added. further remove dcm in vacuo.
this will percipitate the product.
after all dcm removed, solid can be easily collected by filtration. washing with hexanes.

use:
ex: mecn, 3 eq. phosphonium, 60C.