Reaktionsgleichung
[O:1]([C@H:5]1[CH2:10][CH2:9][C@H:8]([NH2:11])[CH2:7][CH2:6]1)[N+:2]([O-:4])=[O:3].[C:12]1(=[O:17])[O:16][CH2:15][CH2:14][CH2:13]1>>[OH:17][CH2:12][CH2:13][CH2:14][C:15]([NH:11][C@H:8]1[CH2:7][CH2:6][C@H:5]([O:1][N+:2]([O-:4])=[O:3])[CH2:10][CH2:9]1)=[O:16]Komponenten
3
Versuchsvorschrift
4.8 g (0.03 mol) trans-4-nitroxycyclohexylamine are mixed with 5.7 ml 4-butyrolactone and stirred for 3 d at room temperature. For the removal of the excess lactone, it is filtered over a silicic gel acid with ethyl acetate. After collection of the pure fractions, it is distilled in a vacuum, triturated with ether and filtered off with suction. There remain 2.1 g of the title compound of the melting point 58°-60° C., i.e. 28% of theory.
Aufarbeitung
- customFor the removal of the excess lactone, it
- filtrationis filtered over a silicic gel acid with ethyl acetate
- customAfter collection of the pure fractions, it
- distillationis distilled in a vacuum
- customtriturated with ether
- filtrationfiltered off with suction
Quellen und Nachweise
- ORD-Eintrag
- ord-804ea5da64ca4972b7c3a4735b112a1e
- Quelldatensatz
- uspto-grants-1995_05
- Patentnummer
- US05411989
Verknüpfte Notizen
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