HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → 1-(2-Hydroxymethylpyrrolidin-1-yl)ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Prolinol | HCID 90908 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(2-Hydroxymethylpyrrolidin-1-yl)ethanone | HCID 550996 | 62.4% |
Reaction Steps
2-(Hydroxymethyl)pyrrolidine (500 mg) was mixed with dichloromethane (5 ml), and TEA (0.9 ml) and acetyl chloride (407 mg) were added thereto at 0° C., followed by stirring at room temperature overnight. 8 M Potassium hydroxide was added to the reaction mixture, followed by stirring at room temperature for 1 hour. The reaction mixture was extracted by the addition of water and CHCl3/MeOH (4:1), the organic layer was washed with water and saturated brine, and dried over anhydrous Na2SO4, and the solvent was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (MeOH/CHCl3) to obtain 1-[2-(hydroxymethyl)pyrrolidin-1-yl]ethanone (442 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08716470B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-79053b708b2d43bbbcdcaa41981c0e39 |
| Source note | uspto-grants-2014_05 |