HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 23467197, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 23467217 | HCID 23467217 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23467197 | HCID 23467197 | — |
Reaction Steps
Sodium hydride (1.2 g of a 50% dispersion in a mineral oil) is added in portions to a stirred solution of 5.4 g of hexahydro-1-phenylspiro[3H-oxazolo[3,4-a]pyridine-3,4'-piperidine] in 100 ml of tetrahydrofuran at 25° C. The mixture is stirred 0.5 hours under nitrogen and 5 g iodomethane in 10 ml of tetrahydrofuran is added dropwise. The mixture is stirred at 45° C. for 3 hours, filtered and the filtrate is evaporated in vacuo. The residue is dissolved in methylene dichloride, washed with water, dried over magnesium sulfate and the solvent is evaporated. The residue is crystallized from ethyl acetate to obtain the desired hexahydro-1'-methyl-1-phenylspiro[3H-oxazolo-[3,4-a]pyridine-3,4'-piperidine]; mp 157°-159° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04260623 |
| Source dataset | uspto-grants-1981_04 |
| ORD ID | ord-4a9e31d0589a40b8ae8504cf3fb8065a |
| Source note | uspto-grants-1981_04 |