Diethyl Ether → HCID 178427636, compound

Participants

Reaction Conditions

Reaction Steps

5.1 g (0.010 mol) of bis(cyclopentadienyl)bis(2,3,5,6-tetrafluoro-4-hydroxyphenyl)titanium are suspended in 100 ml of toluene in a sulfation flask under nitrogen as protective gas. 5.7 g (0.030 mol) of toluene-4-sulfonyl chloride are then added. 40 ml of 1N sodium hydroxide solution (0.040 mol) are subsequently added dropwise, and the mixture is stirred for 4 hours at 40° C. After a check of the reaction using thin-layer chromatography, the reaction mixture is allowed to cool. 100 ml of ice-water and 100 ml of ether are then added. The organic phase is separated off and washed several times with a little water until the reaction on pH paper is neutral. The organic phase is dried using magnesium sulfate and evaporated on a vacuum rotary evaporator. An orange-red crystalline product remains which, after recrystallization from toluene, melts at 226°-228° C.

Provenance & Evidence