HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile--water (1/1) → HCID 24785733, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Reactant | Sodium periodate | HCID 23667635 | — |
| Reactant | HCID 24785465 | HCID 24785465 | — |
| Catalyst | Ruthenium trichloride | HCID 61850 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 24785733 | HCID 24785733 | 68% |
Reaction Steps
Sodium periodate (20 mg) and ruthenium chloride (3 mg) were added to a solution of 3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-5-methyl-4-trifluoromethylthiopyrazole (100 mg), that is described in Example 1, in a mixture of acetonitrile-water (4:1). The reaction mixture was stirred overnight whereupon the mixture was diluted with ethyl acetate and filtered over silica gel. The organic filtrate was washed with water, dried over anhydrous magnesium sulfate, filtered over Celite and concentrated under reduced pressure to give the title compound as a white solid (73 mg, 68%). MS (ES): M/Z [M+H]=452. 1H NMR: (400 MHz, DMSO-d6): 2.46 (s, 3H) and 7.87 (s, 2H). 19F NMR (376 MHz, DMSO-d6): −63.77 (s, 3F) and −79.83 (s, 3F).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09339033B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-d3351322f15845a0af28f6acac117f30 |
| Source note | uspto-grants-2016_05 |