HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chlorobenzenesulfonyl chloride → (2S,4R)-1-t-butoxycarbonyl-4-(4-chlorophenylsulfonylamino)-2-methoxycarbonylpyrrolidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chlorobenzenesulfonyl chloride | HCID 7398 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-tert-butyl 2-methyl (2S,4R)-4-aminopyrrolidine-1,2-dicarboxylate | HCID 7009918 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (2S,4R)-1-t-butoxycarbonyl-4-(4-chlorophenylsulfonylamino)-2-methoxycarbonylpyrrolidine | HCID 14772685 | 88.2% |
Reaction Steps
To a solution of (2S,4R)-4-amino-1-t-butoxycarbonyl-2-methoxycarbonylpyrrolidine (6.04 g) in dichloromethane (60 ml) were added triethylamine (3.44 ml) and p-chlorobenzenesulfonyl chloride (6.26 g) in an ice bath. After being stirred at room temperature overnight, the solution was washed successively with diluted hydrochloric acid, saturated aqueous sodium bicarbonate and brine and dried over magnesium sulfate. The solvent was evaporated in vacuo and the residue was crystallized from n-hexane to give (2S,4R)-1-t-butoxycarbonyl-4-(4-chlorophenylsulfonylamino)-2-methoxycarbonylpyrrolidine (9.13 g) as a pale yellow crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05130323 |
| Source dataset | uspto-grants-1992_07 |
| ORD ID | ord-b3235184275c49ba9703a31a9df8787b |
| Source note | uspto-grants-1992_07 |