Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethyl Acetoacetate | HCID 8868 | — |
| Edukt | Phosphorus trichloride | HCID 24387 | — |
| Edukt | Acetic Acid N'-(3,4-Dichlorophenyl)hydrazide | HCID 612829 | — |
| Produkt | HCID 178429550 | HCID 178429550 | 41,3% |
Reaktionsschritte
To a mixture of (V) (5.0 g, 22.8 mmol) and ethyl acetoacetate (2.97 g 22.8 mmol) was slowly added PCl3 (3.13 g, 22.8 mmol). The mixture was warmed to 50° C. for 1.5 h, poured into ice water (150 ml), and the resulting precipitate was collected on a sintered glass funnel and recrystallized from EtOH to yield (VI) (2.29 g, 41%) as white crystals, mp 208-211° C. (lit. 208-209° C.), TLC CHCl3/MeOH 9:1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08202872B2 |
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| Quelldatensatz | uspto-grants-2012_06 |
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| ORD ID | ord-0c97f8adbe654658923d88615202f0ac |
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| Quellennotiz | uspto-grants-2012_06 |
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