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4-Chloro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline → HCID 22320332、化合物

HRID 497964
ノート
印刷プレビュー

反応式

HRID 497964 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]2[N:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=3)[N:13]=[C:14]([CH3:15])[C:3]=12.O1CCCC1.[CH3:27][NH:28][CH3:29]>O>[CH3:27][N:28]([CH3:29])[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]2[N:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=3)[N:13]=[C:14]([CH3:15])[C:3]=12
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 223201094-Chloro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinolineHCID 22320367Dimethylamine tetrahydrofuran

生成物 1

HCID 22320332HCID 22320332、化合物収率 97.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

4-Chloro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline (1.00 g, 3.39 mmol) was added to a 2M dimethylamine tetrahydrofuran (5.00 mL, 10.0 mmol) solution, and the mixture was heated at 100° C. overnight in a sealed tube. The reaction mixture was cooled to room temperature and poured into water, and organic matter was extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (ethyl acetate to ethyl acetate:methanol=9:1) to give the title compound (1.00 g, 97% yield).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionwas extracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue thus obtained
  7. customwas purified by silica gel column chromatography (ethyl acetate to ethyl acetate:methanol=9:1)

出典と根拠

ORDレコード
ord-d9ddb6e1e5fa45debe62beb1c0d15864
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06949648B2

反応ノート

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