Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | ethyl 4,6-dimethyl-2-oxo-2H-pyran-5-carboxylate | HCID 76918 | — |
| Edukt | Hydrazinium chloride | HCID 115031 | — |
| Lösungsmittel | Potassium Carbonate | HCID 11430 | — |
| Produkt | HCID 58307466 | HCID 58307466 | 7% |
Reaktionsschritte
A mixture of 4,6-dimethyl-2-oxo-2H-pyran-5-carboxylic acid ethyl ester (3.2 mL, 19 mmol) and hydrazine monohydrochloride (1.4 g, 20 mmol) in methanol (16 mL, 0.39 mmol) was heated under microwave irradiation for 2.5 hrs at 150° C. Reaction was taken up in sat. aq. K2CO3 (40 mL) and extracted with ethyl acetate (3×40 mL). The combined organic phases were washed with brine, dried over MgSO4, evaporated and purified by flash chromatography. Yield 7%. 1H NMR (500 MHz, CDCl3): 6.35 (s, 1H), 5.12 (s, 2H), 4.35 (q, J=7.1 Hz, 2H), 2.53 (s, 3H), 2.21 (s, 3H), 1.37 (t, J=7.1 Hz, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08207347B2 |
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| Quelldatensatz | uspto-grants-2012_06 |
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| ORD ID | ord-cafca3c763bb4a119ded67a4451b45ac |
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| Quellennotiz | uspto-grants-2012_06 |
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