HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → (2S,5R)-1-(2-chloroacetyl)-5-ethynylpyrrolidine-2-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | (5R)-1-(chloroacetyl)-5-ethynyl-L-prolinamide | HCID 45081097 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | (2S,5R)-1-(2-chloroacetyl)-5-ethynylpyrrolidine-2-carbonitrile | HCID 16090854 | — |
Reaction Steps
To a stirred solution of (5R)-1-(chloroacetyl)-5-ethynyl-L-prolinamide (0.16 g, 0.745 mmol) and imidazole (0.05 g, 0.745 mmol) in dry pyridine (4 mL) at −35° C. under nitrogen was added POCl3 (0.15 mL, 1.49 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 (CI) m/z 197 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08637546B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-16babfd413a04f1db1e038a033dfc67a |
| Source note | uspto-grants-2014_01 |