Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Potassium Nitrate | HCID 24434 | — |
| Reactant | 1-Propanone, 1-[4-(4-chloro-2-pyridinyl)-1-piperazinyl]-2,2-dimethyl- | HCID 68536990 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 68541591 | HCID 68541591 | — |
Reaction Steps
Dissolve 1-[4-(4-chloro-pyridin-2-yl)-piperazin-1-yl]-2,2-dimethyl-propan-1-one (1.6 mmol, 0.4 g) in sulfuric acid (2.3 mL) and cool the solution down to 0° C. Add potassium nitrate (1.6 mmol, 0.2 g) and stir the mixture allowing to reach room temperature overnight. Dilute the mixture with water and add sodium hydroxide 10% until basic pH. Extract in ethyl acetate. Dry over sodium sulfate, filter, and concentrate under reduced pressure to give a residue of 1-[4-(4-chloro-5-nitro-pyridin-2-yl)-piperazin-1-yl]-2,2-dimethyl-propan-1-one. Subject residue to silica gel chromatography eluting with a mixture hexanes/ethyl acetate as (from 30% up to 60%). MS(ES): m/z=327 [M+H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07652015B2 |
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| Source dataset | uspto-grants-2010_01 |
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| ORD ID | ord-1aac11783ea44614b8182eb9d1330e29 |
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| Source note | uspto-grants-2010_01 |
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