Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | 1H-pyrazol-4-amine | HCID 78035 | — |
| Reactant | HCID 59216810 | HCID 59216810 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 24803453 | HCID 24803453 | — |
Reaction Steps
The title compound was prepared according to general Method B. Thusly, a mixture of trimethylorthoformate (53 mg, 0.50 mmol), acetonitrile (1.5 mL), and 1H-pyrazol-4-ylamine (83 mg, crude, 1.0 mmol) was stirred at 120° C. for 2 hours. After the mixture was cooled to room temperature, 4-Chloro-N-(5-chloro-2-hydrazinocarbonyl-pyridin-3-yl)-3-trifluoromethyl-benzenesulfonamide (42.8 mg, 0.10 mmol) and acetic acid (0.2 mL) was added and the resultant mixture was stirred at 120° C. for 2 hours. After evaporation of solvent under reduced pressure, the residue was further purified through automated normal-phase chromatography and dried (Lyophilizer) to afford title compound. 1H NMR: (DMSO-d6, ppm): 8.90 (s, 1H), 8.08 (m, 2H), 7.90 (m, 2H), 7.80 (m, 2H), 7.75 (m, 1H). MS (ES) [M+H]+ expected 504.0, found 504.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07683176B2 |
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| Source dataset | uspto-grants-2010_03 |
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| ORD ID | ord-06bbf606cc454cde8c2de7da49b78faa |
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| Source note | uspto-grants-2010_03 |
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