Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acrylonitrile | HCID 7855 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-iodopyrazole | HCID 21188126 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21188082 | HCID 21188082 | — |
Reaction Steps
A mixture of 3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-iodopyrazole (0.864 g), acrylonitrile (0.264 g), triethylamine (0.4 ml), palladium acetate (0.04 g) and dimethylformamide (10 ml) were stirred under an atmosphere of nitogen at 70° C. for 24 hours. The reaction mixture was evaporated and the residue partitioned between water and dichloromethane. The organic layer was separated, washed with water, brine, then dried (Na2SO4) and evaporated. The residue was purified by column chromatography on silica gel (40 g) eluted with dichloromethane. Combination and evaporation of suitable fractions gave the title compound as a white solid m.p. 144-145° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06255333B1 |
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| Source dataset | uspto-grants-2001_07 |
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| ORD ID | ord-d5b2184df6814c018e8685680ada8788 |
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| Source note | uspto-grants-2001_07 |
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