HCID 19369824、化合物 → Ethanol, 2-[[2,3-dihydro-1-(4-methoxy-2-methylphenyl)-6-(trifluoromethoxy)-1H-pyrrolo[3,2-c]quinolin-4-yl]amino]-

HRID 849195ノート

反応式

HRID 849195 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[N:10]1[C:22]2[C:21]3[CH:20]=[CH:19][CH:18]=[C:17]([O:23][C:24]([F:27])([F:26])[F:25])[C:16]=3[N:15]=[C:14](Cl)[C:13]=2[CH2:12][CH2:11]1>C(CN)O>[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[N:10]1[C:22]2[C:21]3[CH:20]=[CH:19][CH:18]=[C:17]([O:23][C:24]([F:27])([F:26])[F:25])[C:16]=3[N:15]=[C:14]([NH:15][CH2:16][CH2:17][OH:23])[C:13]=2[CH2:12][CH2:11]1

参加物

3

反応物 1

HCID 19369824HCID 19369824、化合物

生成物 1

HCID 10113707Ethanol, 2-[[2,3-dihydro-1-(4-methoxy-2-methylphenyl)-6-(trifluoromethoxy)-1H-pyrrolo[3,2-c]quinolin-4-yl]amino]-収率 181%

試薬・触媒・溶媒 1

HCID 700Ethanolamine溶媒

反応条件

温度
190 °C

実験手順

1-(2-Methyl-4-methoxyphenyl)-4-chloro-6-trifluoromethoxy-2,3-dihydropyrrolo[3,2-c]quinoline(550 mg, 1.3 mmol) was dissolved in ethanolamine(10 ml) in the pressure tube. The reaction mixture was refluxed at 190° C. for 3 hours. After removing the reaction solvent under reduced pressure, the residue was diluted in dichloromethane(20 ml), and washed with water(15 ml) for 3 times. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography to obtain 510 mg of desired compound as solid in 91% of yield.

後処理

  1. customAfter removing the reaction solvent under reduced pressure
  2. additionthe residue was diluted in dichloromethane(20 ml)
  3. washwashed with water(15 ml) for 3 times
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-ae38b0fb61e643078a1bd012222d6f6e
出典データセット
uspto-grants-2000_01
特許番号
US06011044

反応ノート

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