Reaktionsgleichung
[O:1]([CH2:8][CH2:9][OH:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[N+]([C:16]1[CH:23]=[CH:22][CH:21]=[C:20]([N+:24]([O-:26])=[O:25])[C:17]=1[C:18]#[N:19])([O-])=O>CS(C)=O>[N+:24]([C:20]1[CH:21]=[CH:22][CH:23]=[C:16]([O:10][CH2:9][CH2:8][O:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:17]=1[C:18]#[N:19])([O-:26])=[O:25]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
2-Phenoxyethanol (4.15 ml, 0.033 mole) is added to dimethylsulfoxy sodium prepared from 1.39 g of 57 percent sodium hydride and 40 ml dimethylsulfoxide, giving a mixture of the solid salt of the alcohol after about 20 minutes. This mixture is added to a solution of 5.8 g (0.030 mole) 2,6-dinitrobenzonitrile in 20 ml of dimethylsulfoxide at 30°-40°C., and the resulting purple solution is stirred over night at room temperature. The solvent is removed at 70°C. on a rotary evaporator, and the residue is triturated with water. A solid is filtered off and it is dissolved in ethylacetate. The ethylacetate solution is washed twice with H2O, brine, and dried with calcium sulfate. Evaporation of the ethylacetate, gives 8.5 g of 2-nitro-6(2-phenoxyethyoxy)-benzonitrile, which is crystallized from 200 ml ethyl alcohol, giving 6 g, m.p. 129°-137°C.
Aufarbeitung
- customgiving
- customThe solvent is removed at 70°C. on a rotary evaporator
- customthe residue is triturated with water
- filtrationA solid is filtered off
- dissolutionit is dissolved in ethylacetate
- washThe ethylacetate solution is washed twice with H2O, brine
- dry with materialdried with calcium sulfate
- customEvaporation of the ethylacetate
Quellen und Nachweise
- ORD-Eintrag
- ord-5231937076ce4da885d7c6d317ea8722
- Quelldatensatz
- uspto-grants-1977_07
- Patentnummer
- US04036837
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