HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57942446, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 5-Chloro-3-(4-chloro-3-trifluoromethyl benzenesulfonylamino)-pyridine-2-carboxylic acid | HCID 57942077 | — |
| Reactant | HCID 178418806 | HCID 178418806 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 57942446 | HCID 57942446 | — |
Reaction Steps
A 0° C. mixture of 5-chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carboxylic acid (41 mg, 0.1 mmol, 1 equiv) and 3-aminopyrazole (21 mg, 2.5 equiv) in 0.5 mL of pyridine was treated with 11 μL (1.1 equiv) of POCl3 for 5 minutes. After addition of 1 mL of water, the mixture was subjected to preparative reverse phase HPLC to give 5-chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carboxylic acid (2H-pyrazol-3-yl)-amide. 1H NMR (400 MHz, CDCl3) δ 11.95 (s, 1H), 10.37 (s, 1H), 8.24 (m, 2H), 8.18 (s, 1H), 8.00 (dd, 1H), 7.63 (d, 1H), 7.60 (d, 1H), 6.80 (d, 1H); MS (ES) (M+H)+ expected 480.0, found 480.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08093247B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-540a3604919547a581c812d6317440ac |
| Source note | uspto-grants-2012_01 |