Pyridine → HCID 18403464, Verbindung

HRID 1017210Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1017210
[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([O:8][CH2:9][CH2:10][NH2:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].N1C=CC=CC=1.[C:20](Cl)(=[O:24])[CH:21]([CH3:23])[CH3:22]>C(Cl)Cl.Cl>[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([O:8][CH2:9][CH2:10][NH:11][C:20](=[O:24])[CH:21]([CH3:23])[CH3:22])=[CH:6][CH:5]=1)([O-:3])=[O:2]

Komponenten

6

Edukt 3

HCID 1049PyridineHCID 62325Isobutyryl chlorideHCID 122944662-(4-Nitrophenoxy)ethanamine

Produkt 1

HCID 18403464HCID 18403464, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

2-(4-Nitro-phenoxy)ethylamine (0.27 g) was dissolved in dry DCM (8.5 ml) and dry pyridine (0.15 ml) and isobutyryl chloride (0.12 ml) were then added. After stirring for 1 h at room temperature, the reaction mixture was then diluted with HCl 3 N (50 ml) and extracted with ethyl acetate (50 ml), then the organic phase was washed with brine (50 ml). The organic layer was separated, dried, filtered and evaporated under vacuum to give a crude product which was crystallized (diethyl ether, 7 ml) to give the title compound (0.11 g) as a yellow solid. m.p. 102-103°.

Aufarbeitung

  1. extractionextracted with ethyl acetate (50 ml)
  2. washthe organic phase was washed with brine (50 ml)
  3. customThe organic layer was separated
  4. customdried
  5. filtrationfiltered
  6. customevaporated under vacuum
  7. customto give a crude product which
  8. customwas crystallized (diethyl ether, 7 ml)

Quellen und Nachweise

ORD-Eintrag
ord-a3979d4e05dc4badb73fa6fce8d45f95
Quelldatensatz
uspto-grants-2002_11
Patentnummer
US06479488B1

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