Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | O-(Diphenylphosphinyl)hydroxylamine | HCID 10955453 | — |
| Reactant | Tert-butyl 3-methyl-5-oxopiperazine-1-carboxylate | HCID 22727032 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22727141 | HCID 22727141 | — |
Reaction Steps
tert-Butyl 3-methyl-5-oxo-1-piperazinecarboxylate (1.1 g) was dissolved in DMF (20 ml) and treated with sodium hydride (0.25 g, in oil) with cooling on ice. After stirring at 50° C. for 1 hour, O-diphenylphosphinyl hydroxylamine (1.3 g) was added and the mixture was stirred at 50° C. for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue was combined with aqueous sodium bicarbonate and extracted with dichloromethane. The extract was dried and concentrated to obtain tert-butyl 4-amino-3-methyl-5-oxo-1-piperazinecarboxylate as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06723722B1 |
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| Source dataset | uspto-grants-2004_04 |
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| ORD ID | ord-949b143a25dd4de0a691795ea3f75acd |
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| Source note | uspto-grants-2004_04 |
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