Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diiodomethane | HCID 6346 | — |
| Reactant | Isoamyl Nitrite | HCID 8053 | — |
| Reactant | HCID 17763650 | HCID 17763650 | — |
| Product | HCID 18326232 | HCID 18326232 | — |
Reaction Steps
5.86 g of isoamyl nitrite are added dropwise at a temperature of below 15° C. to a solution of 2.64 g of 3-(5-amino-4-chloro-2-fluoro-phenyl)-4-methyl-5-cyano-1-methyl-[1H]-pyrazole in 54 g (16 ml) of diiodomethane. The reaction mixture is stirred for 14 hours at 22° C., and excess diiodomethane is evaporated in vacuo. All the diiodomethane is subsequently distilled off at 70-75° C./14 torr, and the crude product is purified over a silica gel column (eluent: ethyl acetate/hexane 1/5). The desired product is obtained in a yield of 1.88 g (50.2% of theory).
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-c2e2f7b0070748bd806fd613d8a9e177 |
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| Source note | uspto-grants-2002_01 |
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