Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 6-Chloro-2,4-bis(cyclohexyloxy)pyrimidine | HCID 19006774 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Reactant | HCID 178420582 | HCID 178420582 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178478412 | HCID 178478412 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05340701 |
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| Source dataset | uspto-grants-1994_08 |
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| ORD ID | ord-e80d54d08a1b4776aa1dd49e6e737ba5 |
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| Source note | uspto-grants-1994_08 |
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