Reaktionsgleichung
Br[C:2]1[N:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][CH:3]=1.[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1>C(O)C>[CH3:8][C:6]1[N:7]=[C:2]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[CH:3]=[CH:4][C:5]=1[N+:9]([O-:11])=[O:10]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
To a solution of 6-bromo-2-methyl-3-nitropyridine (2.05 g, 9.45 mmol) in ethanol (10 mL) was added morpholine (1.728 mL, 19.84 mmol) and the reaction mixture was stirred at 70° C. for 5 hours. The reaction mixture was allowed to cool to room temperature causing a precipitate. The solid was collected by filtration and washed with ethanol (5 mL), then dried in vacuo. The crude was redissolved in a mixture of saturated sodium carbonate solution and ethyl acetate. The organic phase was separated, washed with further saturated sodium carbonate solution, then dried over magnesium sulphate and evaporated in vacuo to give the title compound (1.47 g) as a yellow solid. LCMS (2 min, formic) Rt 0.92 min, m/z (ES+) 224 (M+H).
Aufarbeitung
- temperatureto cool to room temperature
- filtrationThe solid was collected by filtration
- washwashed with ethanol (5 mL)
- customdried in vacuo
- dissolutionThe crude was redissolved in a mixture of saturated sodium carbonate solution and ethyl acetate
- customThe organic phase was separated
- washwashed with further saturated sodium carbonate solution
- dry with materialdried over magnesium sulphate
- customevaporated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-456d0803c97f4b36b810f7a4623636de
- Quelldatensatz
- uspto-grants-2016_01
- Patentnummer
- US09242972B2
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