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HCID 19369835、化合物 → HCID 19369810、化合物

HRID 849176
ノート
印刷プレビュー

反応式

HRID 849176 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[C:21]2[C:20]3[CH:19]=[CH:18][CH:17]=[C:16]([O:22][C:23]([F:26])([F:25])[F:24])[C:15]=3[NH:14][C:13](=O)[C:12]=2[CH2:11][CH2:10]1)[CH3:2]>P(Cl)(Cl)(Cl)=O>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[C:21]2[C:20]3[CH:19]=[CH:18][CH:17]=[C:16]([O:22][C:23]([F:25])([F:24])[F:26])[C:15]=3[N:14]=[C:13]([NH:14][CH2:15][CH2:16][OH:22])[C:12]=2[CH2:11][CH2:10]1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 19369835HCID 19369835、化合物

生成物 1

HCID 19369810HCID 19369810、化合物収率 228.8%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

1-(2-Ethylphenyl)-4-oxo-6-trifluoromethoxy-2,3,4,5-tetrahydropyrrolo[3,2-c]quinoline(2.5 g, 6.7 mmol) was dissolved in phosphoryl chloride(10 ml), then the reaction mixture was refluxed for 2 hours. After removing the excess phosphoryl chloride by simple distillation, the residue was poured into iced water, neutralized with aqueous solution of sodium hydroxide(1N), stirred at room temperature for 30 minutes, and extracted with dichloromethane(20 ml) for 3 times. The organic layer was washed with water(15 ml) for 3 times, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography to obtain 3.2 g of desired compound as solid in 85% of yield.

後処理

  1. temperaturethe reaction mixture was refluxed for 2 hours
  2. customAfter removing the excess phosphoryl chloride
  3. distillationby simple distillation
  4. additionthe residue was poured into iced water
  5. extractionextracted with dichloromethane(20 ml) for 3 times
  6. washThe organic layer was washed with water(15 ml) for 3 times
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-a6a6a55ec0174e57a9d5d4a01cf73ea1
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06011044

反応ノート

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