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Methylamine → HCID 19369821, 화합물

HRID 849202
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HRID 849202 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6329MethylamineHCID 19369813HCID 19369813, 화합물

생성물 1

HCID 19369821HCID 19369821, 화합물

반응 조건

온도
180 °C

실험 절차

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.

후처리

  1. customAfter removing the excess solvent
  • distillationby 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
  • 출처 및 근거

    ORD 기록
    ord-e4f96d3c8cde4316aa43ad3c9cfd96dd
    출처 데이터셋
    uspto-grants-2000_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06011044

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