HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → 2-(1-Benzyl-pyrrolidin-3-yl)-5-nitro-pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Benzyl(methoxymethyl)((trimethylsilyl)methyl)amine | HCID 353442 | — |
| Reactant | 2-Ethenyl-5-nitropyridine | HCID 23090550 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(1-Benzyl-pyrrolidin-3-yl)-5-nitro-pyridine | HCID 57470072 | 65.7% |
Reaction Steps
0.15 g of 5-nitro-2-vinyl-pyridine were dissolved in 2.5 ml of dichloromethane, 0.149 g of trifluoroacetic acid (1.31 mmol) were added, followed by slow addition of 0.928 g of N-benzyl-N-(methoxymethyl)-N-trimethylsilylmethylamine (3.91 mmol). Stirring was continued at room temperature for 1 h, before the reaction mixture was washed with aqueous sodium hydrogencarbonate, the aqueous layer reextracted with dichloromethane, the organic layers combined, dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure. The crude product was purified via silica gel chromatography with ethyl acetate. Fractions containing the product were combined, the solvent evaporated to yield 0.186 g of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08470810B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-a2b198619e7f481aa61c15e9355018f7 |
| Source note | uspto-grants-2013_06 |