Water → 2-Chloro-4,5-bis-[(2-methoxyethoxy)-methoxy]-(1,2-epoxy)-styrol
Reaktionsgleichung
C([O:5]O)(C)(C)C.C1(C)C=CC=CC=1.[Cl:14][C:15]1[CH:22]=[C:21]([O:23][CH2:24][O:25][CH2:26][CH2:27][O:28][CH3:29])[C:20]([O:30][CH2:31][O:32][CH2:33][CH2:34][O:35][CH3:36])=[CH:19][C:16]=1[CH:17]=[CH2:18].O>C(Cl)Cl.C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.O=[V]>[Cl:14][C:15]12[O:5][C:16]1([CH:19]=[C:20]([O:30][CH2:31][O:32][CH2:33][CH2:34][O:35][CH3:36])[C:21]([O:23][CH2:24][O:25][CH2:26][CH2:27][O:28][CH3:29])=[CH:22]2)[CH:17]=[CH2:18]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
19 g of vanadylacetylacetonate in solution of 50 ml of methylene chloride were cooled to 0° C. and 3.5 ml of terbutyl hydroperoxide in a toluene solution (3M/l) were added over 30 minutes. The mixture was stirred for 20 minutes at 0° C. and 2.63 g of the product of Stage D in solution in 10 ml of methylene chloride were added. The reaction mixture was stirred for 3 hours at ambient temperature and 30 ml of water were added. The organic phase was separated and the solvent was eliminated under reduced pressure. The residue was chromatographed on silica (eluant: methylene chloride-acetone 8-2) to obtain 21.8 g of the expected product with a Rf=0.35 (CH2Cl2 -acetone 8-2).
Aufarbeitung
- stirringThe reaction mixture was stirred for 3 hours at ambient temperature
- customThe organic phase was separated
- customThe residue was chromatographed on silica (eluant: methylene chloride-acetone 8-2)
Quellen und Nachweise
- ORD-Eintrag
- ord-2ef6f73374884d04a965368627dd044e
- Quelldatensatz
- uspto-grants-1998_06
- Patentnummer
- US05763617
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