Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 18326232 | HCID 18326232 | — |
| Reactant | HCID 178418416 | HCID 178418416 | — |
| Catalyst | HCID 178418476 | HCID 178418476 | — |
| Product | HCID 18326242 | HCID 18326242 | — |
Reaction Steps
5.2 g of 3-(4-chloro-2-fluoro-5-iodophenyl)-4-methyl-5-cyano-1-methyl-[1H]-pyrazole (Example H8), 60 ml of methanol, 2.8 g of triethylamine and 0.4 g of bis(triphenylphosphine)palladium(II) dichloride (PdCl2(PPh3)2) are placed into a 100 ml pressurized container and stirred for 16 hours at a temperature of 100° C. and a carbon monoxide pressure of 10 megapascal (Mpa). The solvent is subsequently evaporated and the crude product which remains is purified over a silica gel column (eluent: ethyl acetate/hexane 1/5). This gives 3.1 g (69.3% of theory) of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06339046B1 |
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| Source dataset | uspto-grants-2002_01 |
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| ORD ID | ord-aad0531215d84836ba9ef4c1ca22ba7a |
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| Source note | uspto-grants-2002_01 |
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