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Acetonitrile → 6-Isopropyl-2-methylimidazo[1,2-b]pyridazine

HRID 1160767
ノート
印刷プレビュー

反応式

HRID 1160767 の反応式
[NH2:1][C:2]1[N:3]=[N:4][C:5]([CH:8]([CH3:10])[CH3:9])=[CH:6][CH:7]=1.Br[CH2:12][C:13](=O)[CH3:14].C(#N)C.[OH-].[Na+]>O>[CH:8]([C:5]1[CH:6]=[CH:7][C:2]2[N:3]([CH:12]=[C:13]([CH3:14])[N:1]=2)[N:4]=1)([CH3:10])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 11715BromoacetoneHCID 14798Sodium HydroxideHCID 230281096-Isopropylpyridazin-3-amine

生成物 1

HCID 230281396-Isopropyl-2-methylimidazo[1,2-b]pyridazine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3-Amino-6-isopropylpyridazine (0.41 g, 2.99 mmol) and bromoacetone (0.53 g, 3.10 mmol) were mixed with acetonitrile (5.0 ml) and heated for 6 hours under reflux. After the reaction was completed, water (20.0 ml) was poured into the reaction solution and adjusted to pH 9 with 20% aqueous sodium hydroxide solution. The reaction solution was extracted twice with ethyl acetate, and the extracts were combined, dried over anhydrous sodium sulfate and concentrated. The residues were purified by silica gel column chromatography (ethyl acetate:chloroform=1:1) to give the title compound as brown oil. The yield was 0.30 g (57.2%).

後処理

  1. temperatureheated for 6 hours
  2. temperatureunder reflux
  3. extractionThe reaction solution was extracted twice with ethyl acetate
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe residues were purified by silica gel column chromatography (ethyl acetate:chloroform=1:1)

出典と根拠

ORDレコード
ord-eb7e0794ddcd429a983eda48e6967952
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07816526B2

反応ノート

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