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3-Amino-1-propanol → HCID 19369772, 화합물

HRID 849204
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HRID 849204 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.[NH2:28][CH2:29][CH2:30][CH2:31][OH:32]>>[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:28][CH2:29][CH2:30][CH2:31][OH:32])[C:11]=2[CH:10]=[CH:9]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 90863-Amino-1-propanolHCID 19369813HCID 19369813, 화합물

생성물 1

HCID 19369772HCID 19369772, 화합물

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온도
180 °C

실험 절차

1-(2-Methylphenyl)-4-chloro-6-β,β,β-trifluoroethoxypyrrolo[3,2-c]quinoline(600 mg, 1.5 mmol), prepared by the procedures of Step 1 and Step 2 in the Example 34, was dissolved in 3-amino-1-propanol(10 ml) in the pressure tube, and the resultant was refluxed at 180° C. for 3 hours. After removing the excess 3-amino-1-propanol 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 522 mg of desired compound as solid in 81% of yield.

후처리

  • customAfter removing the excess 3-amino-1-propanol
  • 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-b8146a79c14c4c6da72e0adb16749501
    출처 데이터셋
    uspto-grants-2000_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06011044

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