tert-Butoxy bis(dimethylamino)methane → beta-Dimethylamino4-methoxy-2,3-dinitrostyrene
Reaktionsgleichung
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH3:9])=[C:5]([N+:10]([O-:12])=[O:11])[C:4]=1[N+:13]([O-:15])=[O:14].[CH3:16][N:17]([CH:19](N(C)C)OC(C)(C)C)[CH3:18]>>[CH3:16][N:17]([CH3:19])[CH:18]=[CH:9][C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([N+:13]([O-:15])=[O:14])[C:5]=1[N+:10]([O-:12])=[O:11]Komponenten
3
Versuchsvorschrift
57.7 g of 4-methoxy-2,3-dinitrotoluene (J. Chem. Soc. 1927:580) is agitated with 150 ml of bisdimethylamino-tert-butoxymethane [Chem. Ber. 101:41 (1968)] for 6 hours at 80° C. After cooling, the precipitated solid material is filtered off, washed with diisopropyl ether, and dried with a water-jet aspirator, thus producing 54.6 g of β-dimethylamino4-methoxy-2,3-dinitrostyrene, mp 100°-131° C.
Aufarbeitung
- temperatureAfter cooling
- filtrationthe precipitated solid material is filtered off
- washwashed with diisopropyl ether