HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Bromoethanol → [1-(2-Hydroxy-ethyl)-piperidin-4-yl]-carbamic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Bromoethanol | HCID 10898 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-(N-Boc-amino)piperidine | HCID 723833 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | [1-(2-Hydroxy-ethyl)-piperidin-4-yl]-carbamic acid tert-butyl ester | HCID 45076484 | 97.3% |
Reaction Steps
2-Bromo-ethanol (2.38 mL, 33.5 mmol, 1.0 eq) is added at room temperature to a stirred solution of piperidin-4-yl-carbamic acid tert-butyl ester (7.0 g, 33.5 mmol, 1.0 eq) in N,N-dimethylformamide (300 mL), followed by potassium carbonate (4.64 g, 33.5 mmol, 1.0 eq). After 6 hours stirring at room temperature, solvent is evaporated and the residue is extracted with ethyl acetate (3×40 mL) and water (40 mL). pH of the aqueous layer is neutralized with a 0.1 N hydrochloric acid aqueous solution. The combined organic layers are dried over sodium sulfate, filtered and concentrated to afford [1-(2-hydroxy-ethyl)-piperidin-4-yl]-carbamic acid tert-butyl ester as an off-white oil (7.96 g, 97% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08927542B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-667a389b225a4962a2bf74e9b7f78efe |
| Source note | uspto-grants-2015_01 |