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HCID 19369788、化合物 → HCID 19369826、化合物

HRID 849184
ノート
印刷プレビュー

反応式

HRID 849184 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=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>P(Cl)(Cl)(Cl)=O>[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[N:9]1[C:21]2[C:20]3[CH:19]=[CH:18][CH:17]=[C:16]([O:22][C:23]([F:24])([F:25])[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
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 19369788HCID 19369788、化合物

生成物 1

HCID 19369826HCID 19369826、化合物収率 162.4%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

1-(2,3-Dimethylphenyl)-4-oxo-6-trifluoromethoxy-2,3,4,5-tetrahydro-pyrrolo[3,2-c]quinoline(4.4 g, 11.8 mmol) was dissolved in phosphoryl chloride(10 ml). 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), and stirred for 30 minutes. The resultant was extracted with dichloromethane(20 ml) for 3 times, and 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 4.0 g of desired compound as solid in 87% 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. extractionThe resultant was extracted 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-78fa2b69f43248b7a1cceb28c12f182d
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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