Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Perfluoro(2-methyl-2-pentene) | HCID 74105 | — |
| Reactant | 3-Chloro-2-hydrazinylpyridine | HCID 556100 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58542581 | HCID 58542581 | — |
Reaction Steps
1.0 g (7.0 mmol) of 3-chloro-2-hydrazinopyridine is suspended in 2.9 ml (21 mmol) of triethylamine and 40.0 ml of acetonitrile and, at −65° C., added to 2.1 g (7 mmol) of (1,1,1,3,4,4,5,5,5-nonafluoro-2-(trifluoromethyl)pent-2-ene. The reaction mixture is slowly heated to room temperature and then stirred at room temperature for 60 hours. The solid is filtered off and afterwashed with diethyl ether. The solvent is removed under reduced pressure on a rotary evaporator. The product is extracted from the residue three times with cyclohexane. The organic phases are combined and the solvent is removed under reduced pressure on a rotary evaporator. This gives 1.95 g of 3-chloro-2-[5-fluoro-3-(pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazol-1-yl]pyridine (73%) as an orange oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08946234B2 |
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| Source dataset | uspto-grants-2015_02 |
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| ORD ID | ord-097dd41f051f4a95afbbf2bd13ffce5c |
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| Source note | uspto-grants-2015_02 |
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