Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromoform | HCID 5558 | — |
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-3-(trifluoromethyl)pyrazole-4-carbonitrile | HCID 10134900 | — |
| Product | HCID 10275860 | HCID 10275860 | — |
Reaction Steps
A stirred mixture of 5-amino-4-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-trifluoromethylpyrazole (3.89 g) and bromoform (13 ml) was treated with tert-butyl nitrite (2.26 ml) at room temperature. After 15 minutes the mixture was heated to 50° C. for 1 hour, and evaporated in vacuo to yield a red oil. This was purified by chromatography on silica (Merck, 40-230 mesh, 0.7 kg cm−2) eluting with a mixture of dichloromethane and petroleum ether (1:2) to furnish 5-bromo-4-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-trifluoromethylpyrazole as a fawn solid m.p. 85-87° C. (3.7 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06372774B1 |
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| Source dataset | uspto-grants-2002_04 |
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| ORD ID | ord-fa77da524975451883e22dcaaa83fc1b |
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| Source note | uspto-grants-2002_04 |
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