HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 3-(Methanesulfonyl-methyl-amino)-pyrrolidine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | tert-Butyl 3-(methylamino)pyrrolidine-1-carboxylate | HCID 45089533 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-(Methanesulfonyl-methyl-amino)-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 66617696 | — |
Reaction Steps
To a solution of 3-methylamino-pyrrolidine-1-carboxylic acid tert-butyl ester (0.50 g) in dichloromethane (10 ml) was added triethylamine (0.38 ml) followed by methanesulfonyl chloride (0.21 ml). After stirring for 24 hours the reaction mixture was diluted with dichloromethane, washed with sodium bicarbonate solution, dried (Mg2SO4) and the solvent removed in vacuo. The residue was purified by flash chromatography to yield 3-(methanesulfonyl-methyl-amino)-pyrrolidine-1-carboxylic acid tert-butyl ester (0.52 g). Treatment of this compound with HCl in dichloromethane/methanol yielded N-Methyl-N-pyrrolidin-3-yl-methanesulfonamide hydrochloride salt (0.41 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08252792B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-6548b9a45733427fbe0bcf273af1d5d0 |
| Source note | uspto-grants-2012_08 |