Reaktionsgleichung
[PH2](O)=O.C(OC)(OC)OC.[PH2:11]([O:13][CH3:14])=[O:12].[N+:15]([C:18]1[CH:25]=[CH:24][C:21]([CH:22]=[CH2:23])=[CH:20][CH:19]=1)([O-:17])=[O:16].C(N(C(C)C)CC)(C)C.C(=O)(O)[O-].[Na+]>CO.O>[CH3:14][O:13][PH:11]([CH2:23][CH2:22][C:21]1[CH:20]=[CH:19][C:18]([N+:15]([O-:17])=[O:16])=[CH:25][CH:24]=1)=[O:12]Komponenten
Edukt 6
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 20 °C
Versuchsvorschrift
0.665 g of crystalline hypophosphorous acid was treated under nitrogen with 1.73 g of trimethyl orthoformate and the mixture was stirred at 20° C. for 2 hours. The resulting solution of crude methyl hypophosphite was added dropwise at 0° C. to a solution of 1 g of 4-nitrostyrene and 0.43 g of diisopropylethylamine in 5 ml of methanol. After 65 hours at 20° C. the same amount of methyl hypophosphite was again added and the mixture was stirred at 20° C. for a further 24 hours. The mixture was diluted with 30 ml of water and the pH was adjusted to 7 with aqueous sodium bicarbonate solution. After extraction with dichloromethane and chromatography on silica gel using 10% methanol in ethyl acetate for the elution there was obtained 0.5 g of 1-[2-(methoxyphosphinyl)ethyl]-4-nitrobenzene in the form of a yellow liquid.
Aufarbeitung
- stirringthe mixture was stirred at 20° C. for a further 24 hours
- extractionAfter extraction with dichloromethane and chromatography on silica gel using 10% methanol in ethyl acetate
- washfor the elution there
Quellen und Nachweise
- ORD-Eintrag
- ord-f4c21074e7fa4b37a69f58637e826285
- Quelldatensatz
- uspto-grants-1988_05
- Patentnummer
- US04743687
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