HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 20306008, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-(4-Hydroxypiperidin-1-yl)ethan-1-one | HCID 10749291 | — |
| Reactant | HCID 20306015 | HCID 20306015 | — |
| Product | HCID 20306008 | HCID 20306008 | 61.8% |
Reaction Steps
N-Acetyl-4-hydroxypiperidine (4.3 g.) in D.M.F. (50 ml.) was added dropwise to a stirred suspension of sodium hydride (3.0 g., 50% dispersion in mineral oil) in D.M.F. (50 ml.) under an atmosphere of nitrogen. After stirring for 3 hours at room temperature 2-[2,6-dimethoxyphenoxy]ethyl mesylate (9.0 g.) in D.M.F. (50 ml.) was added dropwise and stirring continued for 20 hours at room temperature. The solvent was evaporated in vacuo, the residue taken up in water, extracted with chloroform (3×100 ml.), the organic layer dried (Na2SO4) and the solvent evaporated. Distillation gave N-acetyl-4-(2-[2,6-dimethoxyphenoxy]ethoxy)piperidine (6.0 g.), b.p. 200° C. @ 1 mm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04237138 |
| Source dataset | uspto-grants-1980_12 |
| ORD ID | ord-125bac00048e4b1fb7df492330a7f707 |
| Source note | uspto-grants-1980_12 |