Reaktionsgleichung
[NH2:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.[OH-].[K+].Cl[C:12]1[CH:21]=[N:20][C:19]2[C:14](=[CH:15][CH:16]=[C:17]([Cl:22])[CH:18]=2)[N:13]=1.O>CS(C)=O.O1CCOCC1>[Cl:22][C:17]1[CH:18]=[C:19]2[C:14](=[CH:15][CH:16]=1)[N:13]=[C:12]([O:8][C:4]1[CH:3]=[C:2]([CH:7]=[CH:6][CH:5]=1)[NH2:1])[CH:21]=[N:20]2Komponenten
Versuchsvorschrift
6.6 g (0.06 mol) of m-aminophenol in 4.0 g (0.06 mol) of 85% potassium hydroxide and 80 ml of dimethylsulfoxide was heated under stirring. The water generated was distilled away under reduced pressure to make the potassium m-aminophenolate. To the solution which was allowed to cool to room temperature was added a solution of 11.9 g (0.06 mol) of 2,6-dichloroquinoxaline dissolved in 80 ml of dioxane. The mixture was reacted at 50°-60° C. for 5 hours. After the reaction was over, the reaction mixture was poured into ice and cold water. The formed solid was filtered off and washed with 5% aqueous solution of sodium hydroxide and then washed with water. The crude crystals thus obtained were recrystallized from ethanol, to produce 8.8 g (yield 54%) of white crystals, m.p. 119°-120° C.
Aufarbeitung
- distillationThe water generated was distilled away under reduced pressure
- customThe mixture was reacted at 50°-60° C. for 5 hours
- filtrationThe formed solid was filtered off
- washwashed with 5% aqueous solution of sodium hydroxide
- washwashed with water
- customThe crude crystals thus obtained
- customwere recrystallized from ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-13dcfdb62dee414f98a95245d0d21916
- Quelldatensatz
- uspto-grants-1983_03
- Patentnummer
- US04376202
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