Hydrochloric Acid → HCID 69130760, Verbindung
Reaktionsgleichung
[CH3:1][O:2][C:3]1[C:8]([N+:9]([O-])=O)=[CH:7][C:6]([CH3:12])=[CH:5][C:4]=1[N+:13]([O-])=O.[Sn].[ClH:17]>>[ClH:17].[NH2:13][C:4]1[CH:5]=[C:6]([CH3:12])[CH:7]=[C:8]([NH2:9])[C:3]=1[O:2][CH3:1]Komponenten
4
Versuchsvorschrift
2-Methoxy-5-methyl-1,3-dinitrobenzene (0.050 g, 0.236 mmol) was suspended in conc. Hydrochloric acid (1.2 mL). Tin granules (0.118 g, 0.995 mmol) were added slowly to the mixture with stirring at room temperature. After 2 hours, the solution turned white (all the tin granules were dissolved), the solution was cooled to 4° C. The product was collected as a white precipitate and recrystallized from hot water-concentrated hydrochloric acid. Yield=0.037 g (70%) from 0.050 g 2-Methoxy-5-methyl-1,3-dinitrobenzene. White flakes; mp 226° C. (dec); 1H NMR (DMSO) δ: 6.57 (s, 2H), 3.91 (s, broad, 6H), 3.72 (s, 3H), 2.17 (s, 3H).
Aufarbeitung
- dissolutionwere dissolved), the solution
- temperaturewas cooled to 4° C
- customThe product was collected as a white precipitate
- customrecrystallized from hot water-concentrated hydrochloric acid
Quellen und Nachweise
- ORD-Eintrag
- ord-ab1032e0e19f4f00a684b1952f086dab
- Quelldatensatz
- uspto-grants-2008_06
- Patentnummer
- US07384789B2
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