Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromoform | HCID 5558 | — |
| Reactant | Butyl nitrite | HCID 10996 | — |
| Reactant | HCID 21188103 | HCID 21188103 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 21188048 | HCID 21188048 | — |
Reaction Steps
To a stirred solution of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)4-trimethylsilylethynylpyrazole (30 mg, the compound of Example A2) in acetonitrile (0.5 ml) and bromoform (0.5 ml) was added dropwise over five minutes n-butyl nitrite (0.025 ml). The mixture was heated at 70° C. for 30 minutes, then cooled and evaporated. The residue was purified by column chromatography on silica gel (40 g) eluted with dichloromethane: hexane (1:4) to provide the title compound as a white solid m.p. 130° C. (decomp.).
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-25f4428d4eff46c58457942ee357c360 |
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| Source note | uspto-grants-2001_07 |
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