Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 178439462 | HCID 178439462 | — |
| Solvent | Acetonitrile tetrahydrofuran | HCID 22177404 | — |
| Product | HCID 57743079 | HCID 57743079 | 76% |
Reaction Steps
In a 100 ml, three-necked flask fitted with a magnetic stirrer and under inert atmosphere, 1-(1H-imidazol-4-ylmethyl)-4-propylpyrrolidin-2-one 110 (500 mg, 2.4 mmol) is dissolved in a 1/1 mixture of CH3CN/THF (40 ml) and the solution is cooled to 0° C. N-chlorosuccinimide (410 mg, 3.1 mmol) is added by portions while the temperature is maintained at 0° C. The mixture is stirred for 18 h at this temperature. Most of the solvents are removed under vacuum and the residue is dissolved in 1N HCl and diluted with CH2Cl2. The first organic phase is removed and pH of the aqueous phase is adjusted to 9 by addition of solid Na2CO3. Then CH2Cl2 is added and the second organic phase is separated, dried over MgSO4 and concentrated to dryness. Purification by preparative chromatography on silicagel (eluent: CH2Cl2/MeOH/NH4OH: 95/05/0.5 (v/v/v)) affords 440 mg of 1-[(4-chloro-1H-imidazol-5-yl)methyl]-4-propylpyrrolidin-2-one 126.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08586623B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-82da64517f4746e681a4b4428f4bb1ea |
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| Source note | uspto-grants-2013_11 |
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