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

HRID 1663619

反応式

HRID 1663619 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1094202de2f14325bc375ca47f4dffeb
出典データセット
uspto-grants-2011_10
特許番号
US08034812B2

関連ノート

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