Trimethyl orthobeznoate → HCID 12767938, Verbindung
Reaktionsgleichung
[CH3:1][C:2]12[CH2:13][CH2:12][CH:5]([C:6](=[N:10][OH:11])[C:7]1=[N:8][NH2:9])[CH:4]([CH3:14])[O:3]2.CO[C:17](OC)(OC)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>>[C:18]1([C:17]2[N:9]=[N:8][C:7]3[C:2]4([CH3:1])[CH2:13][CH2:12][CH:5]([CH:4]([CH3:14])[O:3]4)[C:6]=3[N+:10]=2[O-:11])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1Komponenten
3
Versuchsvorschrift
A solution of 1.97 g. (0.01 mole) 1,3-dimethyl-2-oxabicyclo[2,2,2]octan-5,6-dione-5-oxime-6-hydrazone in 10 ml. trimethylorthobenzoate is refluxed under nitrogen for 18 hours at a bath temperature of 140° C. during which time all distillate is removed. The resulting mixture is cooled and evaporated to dryness in vacuo. After filtering the residue dissolved in 2% methanol-chloroform through silica gel, and evaporation of the filtrate gives 3-phenyl-5,8-dihydro-6,8-dimethyl-5,8-ethano-6H-pyrano[4,3-e]-as-triazine-4-oxide.
Aufarbeitung
- customis removed
- temperatureThe resulting mixture is cooled
- customevaporated to dryness in vacuo
- filtration