HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Toluenesulfonyl chloride → N-Boc-4-[2-(4-Toluenesulfonyloxy)ethyl]piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-(tert-Butoxycarbonyl)-4-(2-hydroxyethyl)piperidine | HCID 854140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-Boc-4-[2-(4-Toluenesulfonyloxy)ethyl]piperidine | HCID 21936070 | 89.4% |
Reaction Steps
To an ice-cold solution of N-Boc-4-piperidine-ethanol (5.0 g, 21.8 mmol) and Et3N (4.6 mL, 33.0 mmol) in dry DCM (10 mL) was added p-toluenesulfonyl chloride (6.25 g, 32.8 mmol) slowly. Upon addition, the reaction was warmed to room temperature and stirred for 20 h. The reaction mixture was washed with water (40 mL), 10% (wt/v) citric acid(aq) (40 mL), and saturated NaHCO3(aq) (40 mL). The DCM layer was dried with MgSO4, filtered and concentrated in vacuo to give a pale yellow oil, which was chromatographed to give the title compound (7.47 g, 89% yield) as a clear and colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071602B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-bcde2c1edd604a37a9bd7c91469ee2b8 |
| Source note | uspto-grants-2011_12 |