Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 90011140 | HCID 90011140 | — |
| Product | HCID 90011193 | HCID 90011193 | 86% |
Reaction Steps
Step-2: 3-(1-(5-Bromopyridin-2-yl)-5-(trifluoromethyl)-1H-pyrazol-3-yl)-2,2-dimethyl-3-oxopropanehydrazide: A mixture of step-1 intermediate (2.40 g, 5.53 mmol) and hydrazine hydrate (0.87 mL, 27.6 mmol) in ethanol (30 mL) was heated at 80° C. overnight. The reaction mixture was cooled to room temperature and the solvent was then evaporated under vacuum. The residue was triturated with toluene to obtain 2.0 g (86%) of title compound as a white solid. 1HNMR (400 MHz, DMSO-d6) δ 11.78 (s, 1H, D2O exchangeable), 8.72 (d, J=2.0 Hz, 1H), 8.38 (dd, J=2.0 & 8.0 Hz, 1H), 7.92 (d, J=8.0 Hz, 1H), 7.54 (s, 1H), 1.42 (s, 6H); ESI-MS (m/z) 420, 422 [(MH)+, Br79,81].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09409898B2 |
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| Source dataset | uspto-grants-2016_08 |
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| ORD ID | ord-f3f6fdbd62b14c7b875dc0978e6ec4e5 |
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| Source note | uspto-grants-2016_08 |
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