HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 2-Butyl-2-formyl-pyrrolidine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 2-2-Butyl-2-hydroxymethyl-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 66688075 | — |
| Product | 2-Butyl-2-formyl-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 86620858 | 48% |
Reaction Steps
To a stirred solution of 2-2-butyl-2-hydroxymethyl-pyrrolidine-1-carboxylic acid tert-butyl ester (0.763 g, ca. 2.95 mmol) in DCM (30 mL) at 0° C. under nitrogen was added DMP (2.50 g, 5.90 mmol) in a single portion then the reaction mixture was warmed to ambient temperature. After 14 h the reaction mixture was diluted with DCM (70 mL), washed with 1 N NaOH (2×30 mL) and brine (30 mL) then dried (MgSO4), filtered and concentrated in vacuo. Purification by chromatography (silica, 10-20% EtOAc in hexanes) gave 2-butyl-2-formyl-pyrrolidine-1-carboxylic acid tert-butyl ester (0.359 g, 1.41 mmol, 48%) as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08084623B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-8b4ec01406cd46a1a0eff8ebfec8141f |
| Source note | uspto-grants-2011_12 |