HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 68584553, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Reactant | HCID 86630879 | HCID 86630879 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 68584553 | HCID 68584553 | 59% |
Reaction Steps
(4-Amino-5-cyano-2-fluoro-6-methylbiphenyl-3-yl)cyclopentanecarboxylate (I-274) (200 mg, 0.83 mmol) was dissolved in xylene (50 ml), then pyridinium p-toluenesulfonate (50 mg) was added, followed by heating under reflux for 18 hours. After cooling to room temperature, the solvent was evaporated away under reduced pressure. The resulting residue was diluted with ethyl acetate, washed with saturated brine. The obtained organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated away under reduced pressure. The resulting residue was purified by preparative TLC (ethyl acetate:n-hexane=1:2, v/v) to obtain the entitled compound (112 mg, 59%) as a colorless amorphous substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07737166B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-5c887d611f3a483db6c0651dfdb86efb |
| Source note | uspto-grants-2010_06 |