Acetic Anhydride → 1,1-Cyclohexanediacetic Anhydride
Reaktionsgleichung
[C:1]1([CH2:11][C:12]([OH:14])=[O:13])([CH2:7][C:8]([OH:10])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(OC(=O)C)(=O)C>>[C:1]12([CH2:7][C:8](=[O:10])[O:14][C:12](=[O:13])[CH2:11]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2Komponenten
3
Versuchsvorschrift
A suspension of 1,1-cyclohexanediacetic acid (39.95 mmol) in acetic anhydride (159.8 mmol) was refluxed gently until a clear solution was obtained (ca. 1 h). The reaction mixture was kept at reflux for another hour until the reaction was complete. The reaction mixture was cooled to room temperature and acetic acid and excess acetic anhydride were removed under vacuum to afford 7.28 g (100%) of (3). 1H NMR (CDCl3): 2.65 (4H, s); 1.54-1.43 (10H, m).
Aufarbeitung
- temperaturewas refluxed gently until a clear solution
- customwas obtained (ca. 1 h)
- temperatureat reflux for another hour until the reaction
- customacetic acid and excess acetic anhydride were removed under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-2b67861576314e4ebf8b42096805df53
- Quelldatensatz
- uspto-grants-2009_07
- Patentnummer
- US07560483B2
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