Pyrrolidine → 2-(Pyrrolidin-1-yl)pyridin-4-amine

HRID 520493

Reaktionsgleichung

Reaktionsgleichung von HRID 520493
Cl[C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1.[NH:9]1[CH2:13][CH2:12][CH2:11][CH2:10]1>>[N:9]1([C:2]2[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=2)[CH2:13][CH2:12][CH2:11][CH2:10]1

Komponenten

3

Edukt 2

HCID 31268PyrrolidineHCID 844322-Chloropyridin-4-amine

Produkt 1

HCID 452591302-(Pyrrolidin-1-yl)pyridin-4-amineAusbeute 79 %

Reaktionsbedingungen

Temperatur
200 °C

Versuchsvorschrift

A mixture of 2-chloro-4-aminopyridine 109 (2.29 g, 17.8 mmol) and pyrrolidine 68 (5.0 mL) was heated at 200° C. in a microwave reactor for 10 min. After cooling to room temperature, the solid was filtered and washed with dichloromethane (10 mL×3). The filter cake was dissolved in aqueous K2CO3 and extracted with CH2Cl2 (40 mL×3). The combined organic layers were dried over Na2SO4 and concentrated to obtain 110 (2.30 g, 79% yield).

Aufarbeitung

  1. temperatureAfter cooling to room temperature
  2. filtrationthe solid was filtered
  3. washwashed with dichloromethane (10 mL×3)
  4. dissolutionThe filter cake was dissolved in aqueous K2CO3
  5. extractionextracted with CH2Cl2 (40 mL×3)
  6. dry with materialThe combined organic layers were dried over Na2SO4
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-789579a028f04622a9cf2b2cc466a0a5
Quelldatensatz
uspto-grants-2016_05
Patentnummer
US09326986B2

Verknüpfte Notizen

Wird geladen…