HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxybenzenesulfonic acid → HCID 46854533, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxybenzenesulfonic acid | HCID 15619088 | — |
| Reactant | (2S,4S)-1-[2-[(4-ethoxycarbonylbicyclo[2.2.2]oct-1-yl)amino]acetyl]-4-fluoropyrrolidine-2-carboxamide | HCID 46854534 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 46854533 | HCID 46854533 | 81% |
Reaction Steps
(2S,4S)-1-[2-[(4-Ethoxycarbonylbicyclo[2.2.2]oct-1-yl)amino]acetyl]-4-fluoropyrrolidine-2-carboxamide (1.00 g) was dissolved in dichloromethane (10 mL), and a suspension of benzenesulfonic acid monohydrate (500 mg) in dichloromethane-methanol (5:1, 6 mL) was added thereto, followed by stirring at room temperature for 3 hours. The precipitate were collected by filtration, washed with dichloromethane (5 mL) and then dried, thereby obtaining a colorless solid of (2S,4S)-1-[2-[(4-ethoxycarbonylbicyclo[2.2.2]oct-1-yl)amino]acetyl]-4-fluoropyrrolidine-2-carboxamide benzenesulfonate (1.15 g, yield: 81%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08143427B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-ce408b5cadae4ae489ed6b2f07aba731 |
| Source note | uspto-grants-2012_03 |