Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 69074369 | HCID 69074369 | — |
| Catalyst | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| Product | HCID 136199107 | HCID 136199107 | — |
Reaction Steps
2.00 g (4.12 mmol) of 2-[3-(4-chlorophenyl)-4-allyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-N-{-methyl-1-[3-(trifluoromethyl)phenyl]ethyl}-acetamide from Example 371 are dissolved in 20 ml degassed dioxan and treated under argon with 97 mg of tetrakis(triphenylphosphine)-palladium(0) (0.084 mmol), 1.46 ml (10.44 mmol) of triethylamine and 0.32 ml (8.35 mmol) of formic acid and stirred for two hours at 85° C. The suspension is then allowed to cool to room temperature and the precipitated crystals are filtered off at the pump and washed with isopropanol. The mother liquor is concentrated in vacuo and treated with isopropanol, during which further crystals deposit, which are likewise suction-filtered and washed with isopropanol. Together 1.56 g (85% of theory) of the target compound are thus obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08084481B2 |
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| Source dataset | uspto-grants-2011_12 |
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| ORD ID | ord-30a3d39925b04cdcaab6937e688f7cf2 |
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| Source note | uspto-grants-2011_12 |
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