Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phenol | HCID 996 | — |
| Reactant | 4,5,6-Trifluoropyrimidine | HCID 3572764 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | Potassium phenoxide | HCID 23670670 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4,5-Difluoro-6-phenoxypyrimidine | HCID 15869674 | 68.1% |
Reaction Steps
With stirring, 50.4 g (0.45 mol) of potassium tert-butoxide (M=112.22) are added to a solution of 42.4 g (0.45 mol) of phenol in 400 ml of THF. The resulting potassium phenolate solution is added dropwise to a solution of 80 g (0.6 mol) of 4,5,6-trifluoropyrimidine in 1 l of THF which had been cooled to 0° C., and the mixture is stirred for 30 minutes. The solution is concentrated under reduced pressure and the residue is mixed with water and extracted with ethyl acetate. The organic phase is separated off, dried over sodium sulphate and concentrated under reduced pressure. The crude product is stirred with petroleum ether and filtered off. 63.8 g (68.1% of theory) of 5,6-difluoro-4-phenoxypyrimidine of melting point 65-66° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06437127B1 |
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| Source dataset | uspto-grants-2002_08 |
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| ORD ID | ord-2931ca2e58f74826aaec9d0a3d3421a3 |
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| Source note | uspto-grants-2002_08 |
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