HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 68584758, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 178428581 | HCID 178428581 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68584758 | HCID 68584758 | 54.4% |
Reaction Steps
A mixture of N-(5-cyano-2-fluoro-3,3′-dihydroxy-6-methylbiphenyl-4-yl)isobutylamide (I-56) (60 mg, 0.183 mmol), p-toluenesulfonic acid monohydrate (10.4 mg, 0.0548 mmol) and toluene (5 ml) was heated under reflux for 2.5 hours. After cooling, this was diluted with ethyl acetate, successively washed with 1 N hydrochloric acid and saturated brine, dried on anhydrous magnesium sulfate, the solvent was evaporated away under reduced pressure to obtain a pale brown residue. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) to obtain the entitled compound (30.9 mg, 54%) as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07737166B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-0cd8d4294833411bb7c929901a7c1dd2 |
| Source note | uspto-grants-2010_06 |