HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Ammonia
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 1-Carbobenzyloxy-3-phenyl-3-(2-hydroxyethyl)pyrrolidine | HCID 18464926 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ammonia | HCID 222 | 1% |
| Product | 1-Carbobenzyloxy-3-phenyl-3-(2-methanesulfonyloxyethyl)pyrrolidine | HCID 18465104 | — |
Reaction Steps
Combine 1-carbobenzyloxy-3-phenyl-3-(2-hydroxyethyl)pyrrolidine (9.6 g, 29.6 mmol) and triethylamine (8.2 mL, 59.2 mmol) in dichloromethane (150 mL). Cool in an ice-bath. Add methanesulfonyl chloride (2.5 mL, 32.6 mmol). After 16 hours, dilute the reaction mixture with dichloromethane and extract with brine. Dry the organic layer over MgSO4, filter, and evaporate in vacuo to give residue. Chromatograph the residue on silica gel eluting with methanol/dichloromethane 1/10 containing 1% concentrated aqueous ammonia to give 1-carbobenzyloxy-3-phenyl-3-(2-methanesulfonyloxyethyl)pyrrolidine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06194406B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-2e93535b7d984809b0e3f3e213b331f2 |
| Source note | uspto-grants-2001_02 |