HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 4-(1-Methylpyrrolidin-2-yl)benzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 2-(4-Bromophenyl)-1-methylpyrrolidine | HCID 284897 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(1-Methylpyrrolidin-2-yl)benzaldehyde | HCID 86639041 | 74% |
Reaction Steps
To a solution of 2-(4-bromophenyl)-1-methylpyrrolidine (0.45 g, 2 mmol) in dry THF (10 mL) was added dropwise n-BuLi (0.88 mL, 2.2 mmol, 2.5 mol/L in hexane) at −78° C., after the addition was completed the mixture was stirred for 1 h, then dry DMF (0.18 mL, 2.4 mmol) was added to the reaction system and stirring was continued for another 1 hr. Then the reaction mixture was partitioned between EtOAc and 1 N HCl, the aqueous solution was extracted with EtOAc (3×15 mL). The combined organic phase was washed with brine, dried over Na2SO4, and concentrated in vacuo to give crude product (0.28 g, yield 74%) as a yellow oil. The product was used directly in the next step without further purification. LC-MS (ESI) m/z: 189 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08012976B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-57a906eba1284350881daaa2e631882e |
| Source note | uspto-grants-2011_09 |