HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 43215774, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Amino-1-methylpiperidine | HCID 2737531 | — |
| Reactant | Ethyl 4-fluoro-3-nitrobenzoate | HCID 21277355 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 43215774 | HCID 43215774 | — |
Reaction Steps
To a solution of ethyl 4-fluoro-3-nitrobenzoate (2.13 g) and 1-methylpiperidin-4-amine (1.14 g) in tetrahydrofuran (40 mL) was added N,N-diisopropylethylamine (5 mL). The mixture was then stirred at reflux overnight. The solvent was evaporated and the residue was dissolved in ethyl acetate (300 mL) and washed with aqueous NaHCO3, water and brine. After evaporation of the solvent, the residue was dissolved in tetrahydrofuran (20 mL), methanol (10 mL) and water (10 mL). Then, LiOH H2O (2 g) was added. The mixture was stirred at room temperature overnight. The mixture was then concentrated and the residue was neutralized with 5% aqueous HCl. The precipitate was filtered, washed with brine, and dried under vacuum to give the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557983B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-1cf7758faf5a483a98762068fe9b7916 |
| Source note | uspto-grants-2013_10 |