5-(5-Bromopyridin-2(1H)-ylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione → (5-Bromopyridin-2-yl)acetic acid
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[C:8]2C(=O)OC(C)(C)[O:10][C:9]2=[O:17])[NH:6][CH:7]=1>Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([OH:17])=[O:10])=[N:6][CH:7]=1Komponenten
3
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A solution of 5-(5-bromopyridin-2(1H)-ylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3) (40.0 g, 133.3 mmol) in HCl (30%, 400 mL) was heated gently to reflux, and was refluxed for 2 h. The solvent was removed in vacuo and the residue (29.75 g) was used in the next step without further purification. 1H-NMR (CDCl3, 300 MHz): δ 3.79 (s, 2H, CH2), 7.41 (d, 1H, ArH), 8.08 (dd, 1H, ArH), 8.66 (d, 1H, ArH).
Aufarbeitung
- temperatureto reflux
- temperaturewas refluxed for 2 h
- customThe solvent was removed in vacuo
- customthe residue (29.75 g) was used in the next step without further purification
Quellen und Nachweise
- ORD-Eintrag
- ord-ed9b94004346481598f2462e27f3012f
- Quelldatensatz
- uspto-grants-2014_10
- Patentnummer
- US08853258B2
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