Acetic Anhydride → HCID 136338651, Verbindung
Reaktionsgleichung
[C:1]([O:4][C:5](=O)[CH3:6])(=[O:3])[CH3:2].C(N(CC)CC)C.CN(C1C=CC=CN=1)C.[C:24]1([C:34]2[N:39]=[N:38][N:37]=[C:36]([C:40]3[CH:45]=[CH:44][C:43]([O:46]CCO)=[CH:42][C:41]=3[OH:50])[C:35]=2[C:51]2[C:60]3[C:55](=[CH:56][CH:57]=[CH:58][CH:59]=3)[CH:54]=[CH:53][CH:52]=2)[C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH:27]=[CH:26][CH:25]=1>ClCCl>[C:24]1([C:34]2[N:39]=[N:38][N:37]=[C:36]([C:40]3[CH:45]=[CH:44][C:43]([O:46][CH2:6][CH2:5][O:4][C:1](=[O:3])[CH3:2])=[CH:42][C:41]=3[OH:50])[C:35]=2[C:51]2[C:60]3[C:55](=[CH:56][CH:57]=[CH:58][CH:59]=3)[CH:54]=[CH:53][CH:52]=2)[C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH:27]=[CH:26][CH:25]=1Komponenten
6
Versuchsvorschrift
9.11 g of acetic anhydride, 18.1 g of triethylamine and 0.73 g of dimethylaminopyridine in 400 ml of anhydrous dichloromethane are added to the product from Example A9. The reaction mixture is heated to boiling. When the reaction is complete (monitoring by TLC), the solvent is removed in vac. and the residue is taken up in dichloromethane. The organic phase is washed with water and dried with magnesium sulfate. After removal of the solvent, the residue is chromatographed on silica gel, yielding the product having the following NMR data:
Aufarbeitung
- temperatureThe reaction mixture is heated to boiling
- customthe solvent is removed in vac
- washThe organic phase is washed with water
- dry with materialdried with magnesium sulfate
- customAfter removal of the solvent
- customthe residue is chromatographed on silica gel
- customyielding the product
Quellen und Nachweise
- ORD-Eintrag
- ord-32bf5b9791c7448ca1a7e797c6eb1088
- Quelldatensatz
- uspto-grants-2006_08
- Patentnummer
- US07087753B2
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