HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Cyano-N-(3-{6-[1-(4-methoxybenzyl)-1H-pyrazol-4-yl]-3-methyl-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methylphenyl)-5-(pentafluoro-lambda6-sulphanyl)benzamide → 3-Cyano-N-{4-methyl-3-[3-methyl-6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}-5-(pentafluoro-lambda6-sulphanyl)benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Cyano-N-(3-{6-[1-(4-methoxybenzyl)-1H-pyrazol-4-yl]-3-methyl-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methylphenyl)-5-(pentafluoro-lambda6-sulphanyl)benzamide | HCID 89699764 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | 3-Cyano-N-{4-methyl-3-[3-methyl-6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}-5-(pentafluoro-lambda6-sulphanyl)benzamide | HCID 136630238 | — |
Reaction Steps
At 90° C., 115 mg (0.23 mmol) of the compound of Example 56A were stirred in 1.5 ml of trifluoroacetic acid for 60 min. The reaction was then concentrated under reduced pressure and the residue was purified by preparative HPLC (Method 21). The product fractions were combined, concentrated almost completely under reduced pressure and made alkaline with a little saturated aqueous sodium bicarbonate solution. The resulting precipitate was filtered off, washed with water and dried under high vacuum. This gave 60 mg (46% of theory) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09394309B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-5eec758e8fd74c1ebb6da8f08766f27a |
| Source note | uspto-grants-2016_07 |