HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → (2S,5R)-1-(Chloroacetyl)-5-(prop-1-yn-1-yl)pyrrolidine-2-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | (5R)-1-(Chloroacetyl)-5-prop-1-yn-1-yl-L-prolinamide | HCID 66756603 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | (2S,5R)-1-(Chloroacetyl)-5-(prop-1-yn-1-yl)pyrrolidine-2-carbonitrile | HCID 16090855 | — |
Reaction Steps
To a stirred solution of (5R)-1-(chloroacetyl)-5-propynyl-L-prolinamide (0.28 g, 1.23 mmol) and imidazole (0.084 g, 1.23 mmol) in dry pyridine (6 mL) at −35° C. under nitrogen was added POCl3 (0.23 mL, 2.46 mmol) dropwise. The reaction mixture was stirred between −35° C. to −15° C. for 1 hour and evaporated. The residue was diluted with dichloromethane and washed with H2O (2×), dried (Na2SO4), filtered and concentrated under reduced pressure. Purification by flash chromatography (10% ethyl acetate/hexane) provided the titled compound. MS (DCI) m/z 211 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07262207B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-1b6e8d0942864a50b74f59b1b482c2bd |
| Source note | uspto-grants-2007_08 |