1,4-Dioxane → 2-Amino-5-pyridin-3-ylthiophene-3-carbonitrile
Reaktionsgleichung
C(OC(=O)[NH:7][C:8]1[S:9][C:10]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[CH:11][C:12]=1[C:13]#[N:14])(C)(C)C.O1CCOCC1>Cl>[NH2:7][C:8]1[S:9][C:10]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[CH:11][C:12]=1[C:13]#[N:14]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
tert-Butyl(3-cyano-5-pyridin-3-yl-2-thienyl)carbamate (800 mg, 2.07 mmol) was dissolved in 4M hydrochloric acid in dioxane (10.4 ml, 41.6 mmol) and the mixture was stirred at room temperature for 6 h. The mixture was quenched with 1N sodium hydroxide (50 mL) and extracted with ethyl acetate (3×100 mL). The combined organics were dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to afford the title compound as a solid.
Aufarbeitung
- customThe mixture was quenched with 1N sodium hydroxide (50 mL)
- extractionextracted with ethyl acetate (3×100 mL)
- dry with materialThe combined organics were dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-90de99c0f10a42e5893ee2e2ccc47b85
- Quelldatensatz
- uspto-grants-2013_02
- Patentnummer
- US08367706B2
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