Reaktionsgleichung
[Cl-].[Al+3].[Cl-].[Cl-].[Cl:5][CH2:6][CH2:7][C:8](Cl)=[O:9].[CH3:11][C:12]1([CH3:24])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:15]([CH3:23])([CH3:22])[CH2:14][CH2:13]1>C(Cl)Cl>[Cl:5][CH2:6][CH2:7][C:8]([C:19]1[CH:20]=[C:21]2[C:16](=[CH:17][CH:18]=1)[C:15]([CH3:23])([CH3:22])[CH2:14][CH2:13][C:12]2([CH3:24])[CH3:11])=[O:9]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
73.5 g (0.55 mole) of anhydrous aluminum chloride were added a little at a time, at 0°-5° C., to a solution of 70 g (0.55 mole) of 3-chloropropionyl chloride in 200 ml of methylene chloride, after which a solution of 94 g (0.5 mole) of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene in 200 ml of methylene chloride was added dropwise at the same temperature. The mixture was stirred overnight at room temperature, poured onto 1 l of ice/water and extracted with 3 times 300 ml of methylene chloride. The combined organic phases were washed with saturated sodium bicarbonate solution and water, dried over magnesium sulfate and evaporated down. 138 g of 6-(3-chloropropionyl)-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene remained as an oil. The structure was determined by H-NMR spectroscopy.
Aufarbeitung
- extractionextracted with 3 times 300 ml of methylene chloride
- washThe combined organic phases were washed with saturated sodium bicarbonate solution and water
- dry with materialdried over magnesium sulfate
- customevaporated down
Quellen und Nachweise
- ORD-Eintrag
- ord-c751c31d5c6c47d4a0e5e5fb1fe6fa77
- Quelldatensatz
- uspto-grants-1993_04
- Patentnummer
- US05206242
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