Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Methylurea | HCID 11719 | — |
| Reactant | Acetylacetone | HCID 31261 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 853977 | HCID 853977 | — |
Reaction Steps
20.0 g (0.262 mol) of N-methylurea and 29.4 g (0.291 mol) of acetylacetone were together dissolved in 100 ml of absolute ethanol. 97 g of concentrated sulfuric acid were then added, and the reaction mixture heated up. The mixture was then after-stirred for 1 hour at room temperature. After just a short time, the hydrogen sulfate salt of the product precipitated out in the form of a pale, crystalline solid, which was filtered off. This salt was dissolved in a small amount of water and the solution was rendered neutral using 10% strength sodium hydroxide solution. Extraction was then carried out by shaking with chloroform, and the solvent was dried with magnesium sulfate. After removing the solvent on a rotary evaporator, the desired product was produced in the form of pale pink-colored crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07678156B2 |
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| Source dataset | uspto-grants-2010_03 |
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| ORD ID | ord-4f3de9942df5416aa8c8ba1ca29fcd41 |
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| Source note | uspto-grants-2010_03 |
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