Реакция #1829952

Уравнение реакции

biscyclopentadienyltitanium dichloride

water

6-chloro-2,4-bis(cyclohexyloxy)pyrimidine

n-butyllithium

→

title compound

Chlorobis(cyclopentadienyl)(6-chloro-2,4-dicyclohexyloxypyrimidinyl)titanium

Растворители

THF

Условия реакции

Обработка

1. 1
   Температураto warm slowly from -40° C. to 25° C.
2. 2
   Фильтрацияis filtered through ®Hyflo
3. 3
   ДругоеThe aqueous phase is separated off
4. 4
   Другоеthe organic phase is dried
5. 5
   Фильтрацияfiltered
6. 6
   Другоеevaporated on a rotary evaporator
7. 7
   ДругоеThe residue is separated by flash chromatography (SiO2)

Методика

6.15 g (19.8 mmol) of 6-chloro-2,4-bis(cyclohexyloxy)pyrimidine are dissolved in 40 ml of THF under argon as protective gas, the solution is cooled to -40° C., and 12.4 ml of n-butyllithium (1.6M/hexane) are added dropwise. 2.25 g (9 mmol) of solid biscyclopentadienyltitanium dichloride are added to the resultant solution at -40° C. The reaction mixture is allowed to warm slowly from -40° C. to 25° C., is then poured into 40 ml of water and is filtered through ®Hyflo. The aqueous phase is separated off, and the organic phase is dried using magnesium sulfate, filtered and evaporated on a rotary evaporator. The residue is separated by flash chromatography (SiO2), giving 1.0 g of the compound from Example 63 and 0.9 g of the title compound, having a melting range of 145°-155 ° C.

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