HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Fluorophenol → N-tert-butyloxycarbonyl4-(p-fluorophenoxymethyl)piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Fluorophenol | HCID 9732 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | Tert-butyl 4-(hydroxymethyl)piperidine-1-carboxylate | HCID 2764081 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-tert-butyloxycarbonyl4-(p-fluorophenoxymethyl)piperidine | HCID 15512457 | — |
Reaction Steps
Over the course of 30 minutes, 10.5 ml of diethyl azodicarboxylate are poured onto a mixture of 13.5 g of N-tert-butyloxycarbonyl-4-hydroxymethylpiperidine, 7.45 g of p-fluorophenol, 17.4 g of triphenylphosphine and 140 ml of tetrahydrofuran. After stirring for 12 hours at ambient temperature, the reaction mixture is concentrated, taken up in ether, washed with water and then 1N sodium hydroxide solution, and then washed with water. After drying, filtration and evaporation under reduced pressure, chromatography over silica gel (cyclohexane/ethyl acetate: 90/10) allows the expected product to be isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06566364B2 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-2cef51f8c8024ac0bcff6a9554704444 |
| Source note | uspto-grants-2003_05 |