HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 135703014, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Reactant | HCID 18767876 | HCID 18767876 | — |
| Reactant | HCID 18767926 | HCID 18767926 | — |
| Solvent | P-Xylene | HCID 7809 | — |
| Product | HCID 135703014 | HCID 135703014 | — |
Reaction Steps
Ethyl 2-(4-fluorophenyl)-3-oxo-3-(4-pyridyl)-propionate (293 mg, 1.02 mmol), 4-phenylbutanecarboxamidine (315 mg, 1.79 mmol) and pyridinium p-toluenesulfonate (10 mg) were suspended in p-xylene (10 ml). With efficient stirring, the mixture was heated to reflux using a Dean-Stark apparatus with continuous removal of water. After 16 h, the solvent was evaporated and the product purified by column chromatography on silica gel (3% methanol/dichloromethane) followed by recrystallization from acetone. MS (m/z): 400.3 (M+H)+; C25H22FN3O requir. 399.5.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06610698B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-54d0170d2085445092657dfd9e8a8757 |
| Source note | uspto-grants-2003_08 |