HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → 1-(Benzyloxycarbonyl)-4-[(4-nitrophenoxy)methyl]piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | p-Fluoronitrobenzene | HCID 9590 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Benzyl 4-(hydroxymethyl)piperidine-1-carboxylate | HCID 736490 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-(Benzyloxycarbonyl)-4-[(4-nitrophenoxy)methyl]piperidine | HCID 19992422 | — |
Reaction Steps
Sodium hydride (3.36 g of a 50% dispersion in mineral oil) was added portionwise to a stirred solution of the product of part (i) (17.43 g) in dry tetrahydrofuran (200 ml) and the mixture was stirred at room temperature for 1 hour. 4-Fluoronitrobenzene (9.87 g) was added dropwise and the mixture was stirred for a further 18 hours and then evaporated. Water was added to the residue and the mixture was extracted several times with dichloromethane. The combined extracts were washed with water, dried (MgSO4) and evaporated to give an oil which solidified on trituration with ether. The solid was filtered off, washed with a little ether and crystallised from ethyl acetate/hexane to give the product, (13.51 g), m.p. 121°-122°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05057528 |
| Source dataset | uspto-grants-1991_10 |
| ORD ID | ord-28fb6a3c823842c39ae274e0264e68e3 |
| Source note | uspto-grants-1991_10 |