HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21906225, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Reactant | tert-Butyl 4-formylpiperidine-1-carboxylate | HCID 1514430 | — |
| Reactant | 2-amino-N-(5-chloropyridin-2-yl)benzamide | HCID 21906381 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 21906225 | HCID 21906225 | — |
Reaction Steps
A solution containing 1-tert-butoxycarbonyl-4-piperidinecarboxaldehyde (500 mg, 2.34 mmol), 2-amino-N-(5-chloropyridin-2-yl)benzamide (580 mg, 0.23 mmol), and pyridinium p-toluenesulfonate (58 mg, 0.23 mmol) in benzene (250 mL) was heated at reflux with azeotropic removal of water. After 16 h, the mixture was concentrated and the residue partitioned between EtOAc (300 mL) and water (150 mL). The organic phase was separated and washed again with water (150 mL), brine (150 mL); then dried with MgSO4, filtered and concentrated to afford, after purification by column chromatography (SiO2: 0 to 10% EtOAc:methylene chloride), 750 mg (72%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07129245B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-cc897e99d39b4abca319a79e50d6d5e3 |
| Source note | uspto-grants-2006_10 |