Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 2-(Methylamino)ethanol | HCID 8016 | — |
| Edukt | 3-Buten-2-one, 4-(4-hydroxyphenyl)- | HCID 95648 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Sodium Bisulfite | HCID 23665763 | — |
| Produkt | 4-Phenyl-3-Buten-2-one | HCID 15909 | — |
Reaktionsschritte
It should be noted that an initial reaction of 2-methylaminoethanol (1.5 mL) with 4-hydroxybenzylideneacetone (0.68 g) in NaHSO3 (0.78 g) and H2O (1.5 mL) in a sealed vial at 140° C. for 16 hrs did not provide the necessary benzylidene acetone derivative (Scheme 1, compound (b)). Therefore, N-methyl-N-(2-hydroxyethyl)-4-aminobenzaldehyde (Scheme 1, compound (a)) was purchased and used to complete the first step of synthesis instead. When the benzylidene acetone derivative was spotted on a TLC plate the compound glowed fluorescently. The benzylidene acetone derivative reaction mixture was spotted onto preparative TLC plate for purification. Three distinct bands can be observed: a red band at the bottom of the plate, yellow band at the middle, and a faint band at the top were observed. Using mass spectra the inventors determined that the middle yellow band contained the actual benzylidene acetone derivative.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07737183B2 |
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| Quelldatensatz | uspto-grants-2010_06 |
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| ORD ID | ord-31952cbb8ebb4df5a76aaeb5bfb3ec48 |
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| Quellennotiz | uspto-grants-2010_06 |
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