反应详情

6.1 g (0.014 mol) of bis(cyclopentadienyl)bis(2,6-difluoro-3-hydroxyphenyl)titanium and 2.7 g (0.0336 mol) of pyridine in 50 ml of a toluene/DMF mixture (1:1) are introduced into a 100 ml sulfation flask under nitrogen as protective gas. 6.4 g (0.0336 mol) of decanoyl chloride are added dropwise to this red solution at room temperature over the course of 5 minutes, and the mixture is stirred for a further 16 hours (reaction check using thin-layer chromatography). The reaction mixture is then poured into ether and water. The ether phase is evaporated off, washed twice with water, dried using magnesium sulfate and evaporated on a rotary evaporator. The residue is purified by flash chromatography using a hexane/ether mixture 9:1 as eluent, and evaporated on a rotary evaporator. 6.9 g of a red, clear resin are obtained.

1. custom(reaction check using thin-layer chromatography)
2. customThe ether phase is evaporated off
3. washwashed twice with water
4. customdried
5. customevaporated on a rotary evaporator
6. customThe residue is purified by flash chromatography
7. customevaporated on a rotary evaporator
8. custom6.9 g of a red, clear resin are obtained