Reaktionsgleichung
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:18])[C:9]([CH3:17])([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH3:10])=[CH:4][CH:3]=1.[CH2:19]([SH:24])[CH2:20][CH2:21][CH2:22][SH:23].C(=O)([O-])[O-].[K+].[K+].O>CC(N(C)C)=O>[SH:23][CH2:22][CH2:21][CH2:20][CH2:19][S:24][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:18])[C:9]([CH3:17])([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH3:10])=[CH:4][CH:3]=1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
40 g (0.15 mol) of 1-(4-chlorophenyl)-2-methyl-2-morpholin-4-yl-propan-1-one and 109 g (0.89 mol) of 1,4-butanedithiol are dissolved in 300 ml of dimethylacetamide, and the solution is stirred at around 100° C. together with 41 g of potassium carbonate for 5 h. Then the solution is cooled to room temperature and poured into water. The crude product is extracted with ethyl acetate, washed with saturated sodium chloride solution, dried over MgSO4, and concentrated. The residue is purified by column chromatography on silica gel with ethyl acetate -hexane (20:80) as an eluent. Melting point 98 ° C. The structure is confirmed by the 1H-NMR spectrum (CDCl3): δ [ppm] 1.31 (s, 6H), 1.36 (t, 1H), 1.76-1.90 (m, 4H), 2.53-2.62 (m, 6H), 2.98-3.04 (m, 2H), 3.69 (t, 4H), 7.25 (d, 2H), 8.50 (d, 2H).
Aufarbeitung
- extractionThe crude product is extracted with ethyl acetate
- washwashed with saturated sodium chloride solution
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe residue is purified by column chromatography on silica gel with ethyl acetate -hexane (20:80) as an eluent
Quellen und Nachweise
- ORD-Eintrag
- ord-179104a951b34286bb7623e5ec05b593
- Quelldatensatz
- uspto-grants-2000_02
- Patentnummer
- US06022906
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