Ammonium Chloride → 2-Amino-3-(2-methoxycarbonylamino-6-methylbenzyloxy)pyridine

HRID 1762187Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1762187
[Cl-].[NH4+].[CH3:3][O:4][C:5]([NH:7][C:8]1[CH:24]=[CH:23][CH:22]=[C:21]([CH3:25])[C:9]=1[CH2:10][O:11][C:12]1[C:13]([N+:18]([O-])=O)=[N:14][CH:15]=[CH:16][CH:17]=1)=[O:6]>O.C(O)C.[Fe]>[NH2:18][C:13]1[C:12]([O:11][CH2:10][C:9]2[C:21]([CH3:25])=[CH:22][CH:23]=[CH:24][C:8]=2[NH:7][C:5]([O:4][CH3:3])=[O:6])=[CH:17][CH:16]=[CH:15][N:14]=1

Komponenten

6

Edukt 2

HCID 25517Ammonium ChlorideHCID 143684013-(2-Methoxycarbonylamino-6-methylbenzyloxy)-2-nitropyridine

Produkt 1

HCID 200425332-Amino-3-(2-methoxycarbonylamino-6-methylbenzyloxy)pyridine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23925IronKatalysatorHCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a mixture of iron powder (2.76 g) and ammonium chloride (0.275 g) in water (19 ml) and ethanol (63 ml) was added portionwise 3-(2-methoxycarbonylamino-6-methylbenzyloxy)-2-nitropyridine (6.27 g) under reflux and then stirred for an additional 30 minutes. The hot mixture was filtered by suction and the filtrate was made alkaline with sodium bicarbonate and evaporated in vacuo. The residue was washed with water, dried, and recrystallized from ethyl acetate to give 2-amino-3-(2-methoxycarbonylamino-6-methylbenzyloxy)pyridine.

Aufarbeitung

  1. temperatureunder reflux
  2. filtrationThe hot mixture was filtered by suction
  3. customevaporated in vacuo
  4. washThe residue was washed with water
  5. customdried
  6. customrecrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-fa560c57532a489b988757d53d396939
Quelldatensatz
uspto-grants-1989_05
Patentnummer
US04831041

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