Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | HCID 178509105 | HCID 178509105 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178429160 | HCID 178429160 | — |
Reaction Steps
To a mixture of 5-(2-chlorophenyl)-4-(4-chlorophenyl)-2H-pyrazol-3-ylamine (I-3A-1b; 3.00 g, 9.86 mmol) in acetic acid (12 ml) was added ethyl acetoacetate (1.63 ml, 12.8 mmol). The reaction was heated at 100° C. for 16 hours. After cooling to room temperature, the precipitated solid was isolated by vacuum filtration and then repulped from diethyl ether to afford I-3A-4a (1.1 g, 30%) as a colorless solid: +ESI MS (M+1) 370.0; 1H NMR (400 MHz, DMSO-d6) δ 12.12 (s, 1H), 7.45–7.33 (m, 6H), 7.13 (d, J=8.7 Hz, 2H), 5.70 (s, 1H), 2.30 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07176210B2 |
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| Source dataset | uspto-grants-2007_02 |
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| ORD ID | ord-6ee709fdac5f4ba09afe57ddd2961c14 |
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| Source note | uspto-grants-2007_02 |
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