Diethyl Ether → 6-Iodoimidazo[1,2-B]pyridazin-2-amine

HRID 1663619

Reaktionsgleichung

Reaktionsgleichung von HRID 1663619
[I:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([NH:11]C(=O)OC(C)(C)C)[N:10]=2)[N:7]=1.Cl.C(OCC)(=O)C.C(OCC)C>C(OCC)(=O)C>[I:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([NH2:11])[N:10]=2)[N:7]=1

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 21866389Hydrogen chloride-ethyl acetateHCID 46941915Tert-butyl (6-iodoimidazo[1,2-b]pyridazin-2-yl)carbamate

Produkt 1

HCID 574410246-Iodoimidazo[1,2-B]pyridazin-2-amineAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a suspension of tert-butyl (6-iodoimidazo[1,2-b]pyridazin-2-yl)carbamate (10.2 g, 28.3 mmol) in ethyl acetate (50 mL) was added 4N hydrochloric acid/ethyl acetate (75 mL), and the mixture was stirred at room temperature for 4 hr. Diethyl ether (200 mL) was added to the reaction mixture, and the precipitate was filtrated. After washing with saturated aqueous sodium hydrogencarbonate solution, the filtrate was washed with water, acetonitrile and diethyl ether to give the title compound (4.9 g, 67%) as a green powder.

Aufarbeitung

  1. filtrationthe precipitate was filtrated
  2. washAfter washing with saturated aqueous sodium hydrogencarbonate solution
  3. washthe filtrate was washed with water, acetonitrile and diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-1094202de2f14325bc375ca47f4dffeb
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08034812B2

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