HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-[(6-Chloro-2-naphthyl)sulfonyl]-1-[methyl[1-(2-methyl-4-pyridinyl)-4-piperidinyl]amino]-6-oxo-2-piperazinecarboxylic Acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22727060 | HCID 22727060 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 4-[(6-Chloro-2-naphthyl)sulfonyl]-1-[methyl[1-(2-methyl-4-pyridinyl)-4-piperidinyl]amino]-6-oxo-2-piperazinecarboxylic Acid | HCID 22727105 | 84.1% |
Reaction Steps
A mixture of methyl 4-[(6-chloro-2-naphthyl)sulfonyl]-1-[methyl[1-(2-methyl-4-pyridinyl)-4-piperidinyl]amino]-6-oxo-2-piperazinecarboxylate hydrochloride (0.22 g) obtained in Example 128 and a 1N aqueous solution of sodium hydroxide (1.4 ml) in methanol (4.0 ml) was stirred at 40° C. for 30 minutes. The reaction mixture was cooled, and the reaction system was adjusted at pH 5 with 1N hydrochloric acid, and then concentrated under reduced pressure. The residue was purified on a CHP-20 column (water→1% conc. aqueous ammonia-containing 25% aqueous solution of acetonitrile) to obtain the title compound (0.17 g) as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06723722B1 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-7ae1d2305b7d473382d3a38497a02f55 |
| Source note | uspto-grants-2004_04 |