Pyrrolidine → HCID 18953550, Verbindung

HRID 1491639Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1491639
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[NH:11]1[CH2:15][CH2:14][CH2:13][CH2:12]1>O1CCOCC1>[N:11]1([C:2]2[CH:7]=[CH:6][N:5]=[CH:4][C:3]=2[N+:8]([O-:10])=[O:9])[CH2:15][CH2:14][CH2:13][CH2:12]1

Komponenten

4

Edukt 2

HCID 31268PyrrolidineHCID 27357814-Chloro-3-nitropyridine

Produkt 1

HCID 18953550HCID 18953550, VerbindungAusbeute 95,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

4-Chloro-3-nitropyridine (2.02 g, 12.7 mmol) was suspended in 15 ml of 1,4-dioxane. The suspension was cooled a little in an ice bath, and then pyrrolidine (2.1 ml, 25.3 mmol ) was added dropwise thereto. The temperature of the suspension was returned to room temperature, and the suspension was stirred for 30 minutes, followed by removal of the solvent by distillation under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate) to obtain 2.34 g of a yellow solid (yield: 95.4%).

Aufarbeitung

  1. temperatureThe suspension was cooled a little in an ice bath
  2. customwas returned to room temperature
  3. customfollowed by removal of the solvent by distillation under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-928ee9d366bd43698562826f1125db26
Quelldatensatz
uspto-grants-1994_12
Patentnummer
US05371086

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