HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → Benzyl 3-formylpyrrolidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | Benzyl 3-(hydroxymethyl)pyrrolidine-1-carboxylate | HCID 18332648 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Benzyl 3-formylpyrrolidine-1-carboxylate | HCID 4620242 | — |
Reaction Steps
DMSO (597 μL, 8.42 mmol) was added to a solution of oxalyl chloride (427 μL, 5.05 mmol) in DCM (25 mL) at −78° C. After 5 minutes, benzyl 3-(hydroxymethyl)pyrrolidine-1-carboxylate (generated in Step 1) was added. The reaction was continued for 30 minutes at −78° C. TEA (2.3 mL, 17 mmol) was then added. The resulting mixture was then allowed to warm to room temperature over the course of 30 minutes. Water was then added. The layers were separated and the organic phase was washed sequentially with 0.1 N HCl, water, saturated NaHCO3, and brine. The organic phase was then dried over sodium sulfate and the solvent was removed in vacuo to afford the product (0.82 g, 88% over two steps).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08530485B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-5e0b1f53aca24c0aa0fe85932caf779b |
| Source note | uspto-grants-2013_09 |