HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfide → 1-Benzyl 3-ethyl 3-(2-oxoethyl)piperidine-1,3-dicarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfide | HCID 1068 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ozone | HCID 24823 | — |
| Reactant | 1-Benzyl 3-ethyl 3-(3-methylbut-2-en-1-yl)piperidine-1,3-dicarboxylate | HCID 59868918 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-Benzyl 3-ethyl 3-(2-oxoethyl)piperidine-1,3-dicarboxylate | HCID 59868916 | — |
Reaction Steps
Ozone was passed through a solution of 1-benzyl 3-ethyl 3-(3-methylbut-2-en-1-yl)piperidine-1,3-dicarboxylate (35.2 g, 0.0979 mol) in methylene chloride (800 mL) at −78° C. until the color of the solution turned blue. The reaction mixture was then flushed with nitrogen until the blue color dissipated. Dimethylsulfide (Aldrich, cat #: 274380) (14 mL, 0.19 mol) and triethylamine (26.5 mL, 0.19 mol) were added and the mixture was stirred at ambient temperature overnight. The volatile solvent were removed under reduced pressure and purified directly by flash chromatography on a silica gel column with 20% ethyl acetate in hexanes to afford the desired product in quantitative yield. LC/MS 334.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006260B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-10b5ffa36a8b44a09e07c0ccce50e766 |
| Source note | uspto-grants-2015_04 |