Sodium Carbonate → HCID 22024220, Verbindung

HRID 1792753Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1792753
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][OH:7].Cl[C:9]1[CH:14]=[CH:13][N:12]=[N:11][C:10]=1[Cl:15].C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1>[Cl:15][C:10]1[N:11]=[N:12][C:13]([NH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][OH:7])=[CH:14][CH:9]=1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 756345-Aminopentan-1-olHCID 2521503,4-dichloropyridazine

Produkt 1

HCID 22024220HCID 22024220, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of 5-amino-1-pentanol (433 mg, 4.2 mmol), dichloropyridazine (1.25 g, 8.39 mmol) and sodium carbonate (890 mg, 8.39 mmol) was stirred in 1,4-dioxane (40 ml) and heated at 70-80° for 3 days under an atmosphere of argon. The solvent was removed under reduced pressure and the residue was partitioned between dichloromethane (300 ml) and water (38 ml). The organic layer was separated, dried and concentrated to give an orange solid which was chromatographed on silica, using hexane/ethyl acetate (1:1). The product, 5-(6chloro-3-pyridazinyl)amino-1-pentanol was isolated as a pale yellow solid (202 mg, 22%).

Aufarbeitung

  1. temperatureheated at 70-80° for 3 days under an atmosphere of argon
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was partitioned between dichloromethane (300 ml) and water (38 ml)
  4. customThe organic layer was separated
  5. customdried
  6. concentrationconcentrated
  7. customto give an orange solid which
  8. customwas chromatographed on silica

Quellen und Nachweise

ORD-Eintrag
ord-7b93615a1aee4f05861c3a6bb484f95d
Quelldatensatz
uspto-grants-2006_07
Patentnummer
US07078403B1

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