Reaktionsgleichung
[CH3:1][O:2][C:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]=1.[N:9](OC)=[O:10].B(F)(F)F.C[CH2:18][O:19]CC.[S:22](=[O:24])=[O:23]>>[CH3:1][O:2][C:3]1([O:19][CH3:18])[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]1[N:9]=[O:10].[S:22](=[O:24])=[O:23]Komponenten
Versuchsvorschrift
1,1-Dimethoxy-2-nitrosocyclohexane dimer was prepared as described in Example 1 from 1-methoxycyclohexene (46.8 g., 0.417 mole), methyl nitrite (30.6 g., 0.501 mole) and boron trifluoride-etherate (0.25 ml., 0.28 g., 2.0 × 10-3 mole) in 250 ml. of sulfur dioxide. The crude nitroso dimer, 76.0 g. of a gummy yellow-green solid still containing traces of sulfur dioxide, was obtained by the method described earlier. Without purification, the dimer was subjected to isomerizing conditions in methanol/sodium methoxide solution. Filtration through celite (to remove colloidal solids that had formed) and evaporation afforded 66.0 g. of an off-white slightly moist solid. Recrystallization from 180 ml. of ether at -70° C. gave 26.8 g. (37.2%) of 1,1-dimethoxy-2-oximinocyclohexane as colorless fine needles, m.p. 112°-116° C. An additional 2.9 g. (4.0%) of slightly impure oxime was obtained from the mother liquor as a white powder, m.p. 105°-112° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-4c0d740083164e6c8a559e8a92617511
- Quelldatensatz
- uspto-grants-1977_08
- Patentnummer
- US04045422
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