Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Cyanide | HCID 8929 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 18768940 | HCID 18768940 | — |
| Reactant | Ammonia methanol | HCID 21705897 | — |
| Product | HCID 18768930 | HCID 18768930 | 51% |
Reaction Steps
To a dry 250 mL round bottom flask set with a condenser was added sodium cyanide (0.786 g, 16.03 mmol), ammonium chloride (0.904 g, 16.9 mmol) and NH3/MeOH (2.0 M, 15.36 mL, 30.7 mmol). To the mixture was added 1-(3,3-dimethyl-butyl)-pyrrolidin-3-one (2.60 g, 15.36 mmol) and MgSO4 (2.5 g). The mixture was heated at 60° C. in an oil bath and stirred for 4 h. The mixture was cooled to room temperature and filtered to remove the insolubles, the filtrate was concentrated to dryness and the residue was dissolved in EtOAc/Et2O and filtered through a pad of diatomaceous earth then concentrated to dryness to give the title compound in (1.5 g, 51% yield). The crude compound was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06649642B2 |
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| Source dataset | uspto-grants-2003_11 |
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| ORD ID | ord-8ab3e44a279f4a94a9efcd4c5fe07f72 |
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| Source note | uspto-grants-2003_11 |
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