Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Acetylacetone | HCID 31261 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Product | HCID 178468373 | HCID 178468373 | 96% |
Reaction Steps
Variant a): In a stirred vessel, 21 l of 20% strength sulfuric acid and 6 kg (60 mol) of acetylacetone were initially charged. The mixture was cooled to about 17° C. and, at 15-20° C., 4.2 kg (60.84 mol) of 40.5% strength aqueous sodium nitrite solution were metered in. The mixture was subsequently stirred at about 17° C. for another 20 minutes and then extracted with 25 l of ethyl acetate. The organic phase was concentrated under reduced pressure, giving 7.42 kg (96% yield) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06441236B1 |
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| Source dataset | uspto-grants-2002_08 |
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| ORD ID | ord-93fb51ce83c846e2a2bdbc192965c9c3 |
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| Source note | uspto-grants-2002_08 |
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