HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → (2-Ethoxycarbonyl)-(1-formyl)ethylene oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | Ethyl acetate pentane | HCID 22335286 | — |
| Reactant | (2-Ethoxycarbonyl)-(1-hydroxymethyl) ethylene oxide | HCID 88418003 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | (2-Ethoxycarbonyl)-(1-formyl)ethylene oxide | HCID 88418014 | 80% |
Reaction Steps
The procedure described by Evans and Williams European Patent Application No. 89302778.9, Publication No. 0334593 was employed for the Swern oxidation of (2-ethoxycarbonyl)-(1-hydroxymethyl) ethylene oxide (5.00 g) in methylene chloride (total 170 ml) with dimethylsulfoxide (7.3 mL), oxalyl chloride (4.2 mL) and triethylamine. Extractive work-up involving brine (150 mL), followed by trituration of impurities with pentane-ethyl acetate (2:1, 450 mL) afforded the title aldehyde (4.0 g, 80%). This material is used immediately and/or stored in dry methylene chloride at -25° C. under nitrogen.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05391728 |
| Source dataset | uspto-grants-1995_02 |
| ORD ID | ord-93295231ae79499b87ab4a483dfec7c3 |
| Source note | uspto-grants-1995_02 |