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

HRID 1946451
ノート
印刷プレビュー

反応式

HRID 1946451 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-2355043a2e7c4b6984281c8ea170aea4
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399381B2

反応ノート

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