Water → 2-[(5,6-Dihydro-[1,4,2]dioxazin-3-yl)-methoxyimino-methyl]-benzaldehyde
Reaktionsgleichung
C[N+]1([O-])CC[O:5]CC1.[CH3:9][O:10][N:11]=[C:12]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[CH2:25]Cl)[C:13]1[O:18][CH2:17][CH2:16][O:15][N:14]=1.O>CN(C)C=O>[O:15]1[CH2:16][CH2:17][O:18][C:13]([C:12](=[N:11][O:10][CH3:9])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[CH:25]=[O:5])=[N:14]1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
19.5 g (0.14 mol) of N-methylmorpholine N-oxide are added to a solution of 15 g (0.056 mol) of (2-chloromethyl-phenyl)-(5,6-dihydro-[1,4,2]dioxazin-3-yl)-methanone O-methyl oxime in 150 ml of dimethylformamide and the mixture is stirred at 120° C. for 2 hours. After cooling, the mixture is poured into 1000 ml of water and extracted three times with 200 ml of ethyl acetate each time. The combined organic phases are dried over magnesium sulphate and concentrated under reduced pressure. The residue is stirred with diisopropyl ether and the solid formed is filtered off with suction. 10.5 g (76% of theory) of 2-[(5,6-dihydro-[1,4,2]dioxazin-3-yl)-methoxyimino-methyl]-benzaldehyde are obtained.
Aufarbeitung
- temperatureAfter cooling
- extractionextracted three times with 200 ml of ethyl acetate each time
- dry with materialThe combined organic phases are dried over magnesium sulphate
- concentrationconcentrated under reduced pressure
- stirringThe residue is stirred with diisopropyl ether
- customthe solid formed
- filtrationis filtered off with suction
Quellen und Nachweise
- ORD-Eintrag
- ord-55ce8ac9ef244f81b2349ddb2fb10a33
- Quelldatensatz
- uspto-grants-2002_07
- Patentnummer
- US06420362B1
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