反应详情

8.7 g (0.020 mol) of bis(cyclopentadienyl)bis(2,6-difluoro-3-hydroxyphenyl)titanium and 3.8 (0.048 mol) of pyridine in 30 ml of toluene/DMF mixture (1:1) are introduced into a 100 ml sulfation flask under nitrogen as protective gas. 4.9 g (0.048 mol) of acetic anhydride are added dropwise to this solution at room temperature over the course of 5 minutes, and the mixture is stirred for a further 24 hours (reaction check using thin-layer chromatography). The reaction mixture is then poured into ether and water. The ether phase is separated off, washed three times with water, dried using magnesium sulfate and evaporated on a rotary evaporator. The residue is purified by flash chromatography using a hexane/ether mixture 1:1 and, after evaporation, crystallized from an ether/hexane mixture. 7.7 g of a yellow powder of melting point 104°-123° C. (decomposition) are obtained.

1. custom(reaction check using thin-layer chromatography)
2. customThe ether phase is separated off
3. washwashed three times with water
4. customdried
5. customevaporated on a rotary evaporator
6. customThe residue is purified by flash chromatography
7. customafter evaporation
8. customcrystallized from an ether/hexane mixture