Reaktionsgleichung
[CH2:1]([C:3]([OH:18])([C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:25]([N:28]([CH2:32][CH2:33][CH2:34]Cl)[CH2:29][CH2:30][CH3:31])[CH2:26][CH3:27]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C>[CH2:1]([C:3]([OH:18])([C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:4]1[CH:5]=[CH:6][C:7]([O:10][CH2:27][CH2:26][CH2:25][N:28]([CH2:32][CH2:33][CH3:34])[CH2:29][CH2:30][CH3:31])=[CH:8][CH:9]=1)[CH3:2]Komponenten
6
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
13.1 g. of α-ethyl-α-(4-chlorophenyl)-4-hydroxy-benzylalcohol, 14 g. of anhydrous potassium carbonate, 9.8 g. of dipropylaminopropyl chloride and 0.85 g. of tetrabutyl ammonium hydrogensulfate in 135 ml. of ethyl acetate are slightly boiled for 20 hours, under stirring. After cooling the mixture, the solvent is evaporated in vacuo. To the residue water and benzene are added. The phases are separated, the benzene solution is washed with water, dried over anhydrous potassium carbonate, filtered and evaporated. The residue is purified by vacuum fractionation. 13.8 g. of the desired end product are obtained, boiling at 198° to 200° C./1.33 Pa.
Aufarbeitung
- temperatureAfter cooling the mixture
- customthe solvent is evaporated in vacuo
- additionTo the residue water and benzene are added
- customThe phases are separated
- washthe benzene solution is washed with water
- dry with materialdried over anhydrous potassium carbonate
- filtrationfiltered
- customevaporated
- customThe residue is purified by vacuum fractionation
- customof the desired end product are obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-207e32b5a3714d40af02fe0ad4959c98
- Quelldatensatz
- uspto-grants-1987_02
- Patentnummer
- US04645779
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