HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → N-(5-Chloropyridin-2-yl)-2-[(1-isopropylpiperidin-4-ylcarbonyl)amino]-4-methoxycarbonylbenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 1-Isopropylpiperidine-4-Carboxylic Acid | HCID 6484187 | — |
| Reactant | 2-amino-N-(5-chloropyridin-2-yl)-4-methoxycarbonylbenzamide | HCID 21906318 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-(5-Chloropyridin-2-yl)-2-[(1-isopropylpiperidin-4-ylcarbonyl)amino]-4-methoxycarbonylbenzamide | HCID 21906664 | 52% |
Reaction Steps
A solution of 1-isopropylpiperidine-4-carboxylic acid (2.0 g, 9.6 mmol) in methylene chloride (70 mL) was treated dropwise with thionyl chloride (0.70 mL, 9.6 mmol). After heating to reflux for 1 h, 2-amino-N-(5-chloropyridin-2-yl)-4-methoxycarbonylbenzamide (1.5 g, 4.8 mmol) was added. After 0.5 h, pyridine (0.80 mL) was added and the resulting mixture heated at reflux. After 12 h, the mixture was cooled, treated with water, 1 N NaOH (20 mL), and concentrated. The residue was purified by column chromatography (SiO2: 5% methanol:methylene chloride) affording 1.14 g (52%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06635657B1 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-903c31855b404beaacb1f861b75fe92a |
| Source note | uspto-grants-2003_10 |