HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (R)-N,N-Dimethyl-1-(4-nitro-2-(trifluoromethyl)benzyl)pyrrolidin-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (3R)-(+)-3-(Dimethylamino)pyrrolidine | HCID 2758521 | — |
| Reactant | 1-(Bromomethyl)-4-nitro-2-(trifluoromethyl)benzene | HCID 46838761 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (R)-N,N-Dimethyl-1-(4-nitro-2-(trifluoromethyl)benzyl)pyrrolidin-3-amine | HCID 66735770 | 60.3% |
Reaction Steps
To a solution of crude 1-(bromomethyl)-4-nitro-2-(trifluoromethyl)benzene (17.5 mmol, 75% pure) in 40 mL of DCM was added Et3N (2.69 mL, 19.3 mmol) and (R)-(+)-3-(dimethylamino)pyrrolidine (2.0 g, 17.5 mmol). After stirring overnight at ambient temperature under an atmosphere of N2, the reaction solution was concentrated, added aq. NaHCO3 (100 mL), and the resulting mixture extracted with DCM (4×50 mL). The combined organic layer was dried over Na2SO4, filtered, concentrated, and the resulting residue was purified by silica gel chromatography (eluted with 0-10% MeOH/DCM) to provide 3.35 g of product as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029533B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-032070bbef4b4cdf836b5724bfc3d2e9 |
| Source note | uspto-grants-2015_05 |