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Methylamine → HCID 19369821、化合物

HRID 849202
ノート
印刷プレビュー

反応式

HRID 849202 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:20]2[C:19]3[CH:18]=[CH:17][CH:16]=[C:15]([O:21][CH2:22][C:23]([F:26])([F:25])[F:24])[C:14]=3[N:13]=[C:12](Cl)[C:11]=2[CH:10]=[CH:9]1.[CH3:28][NH2:29]>>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:20]2[C:19]3[CH:18]=[CH:17][CH:16]=[C:15]([O:21][CH2:22][C:23]([F:26])([F:25])[F:24])[C:14]=3[N:13]=[C:12]([NH:29][CH3:28])[C:11]=2[CH:10]=[CH:9]1
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

3

反応物 2

HCID 6329MethylamineHCID 19369813HCID 19369813、化合物

生成物 1

HCID 19369821HCID 19369821、化合物

反応条件

温度
180 °C

実験手順

1-(2-methylphenyl)-4-chloro-6-β,β,β-trifluoroethoxypyrrolo[3,2-c]quinoline(600 mg, 1.5 mmol) was dissolved in aqueous solution of methylamine(40%, 10 ml) in the pressure tube, and the resultant was refluxed at 180° C. for 3 hours. After removing the excess solvent by distillation 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 446 mg of desired compound as solid in 77% of yield.

後処理

  1. customAfter removing the excess solvent
distillation
by distillation under reduced pressure
  • additionthe residue was diluted in dichloromethane(20 ml)
  • washwashed with water(15 ml) for 3 times
  • dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  • filtrationfiltered
  • concentrationconcentrated under reduced pressure
  • customThe residue was purified by silica gel chromatography
  • 出典と根拠

    ORDレコード
    ord-e4f96d3c8cde4316aa43ad3c9cfd96dd
    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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