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HCID 19369825, 화합물 → HCID 19369826, 화합물

HRID 849185
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HRID 849185 반응식
[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[N:14]=[C:13](Cl)[C:12]=2[CH2:11][CH2:10]1>C(CN)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:26])([F:25])[F:24])[C:15]=3[N:14]=[C:13]([NH:14][CH2:15][CH2:16][OH:22])[C:12]=2[CH2:11][CH2:10]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 19369825HCID 19369825, 화합물

생성물 1

HCID 19369826HCID 19369826, 화합물수율 140.1%

시약·촉매·용매 1

HCID 700Ethanolamine용매

반응 조건

온도
190 °C

실험 절차

1-(2,3-Dimethylphenyl)-4-chloro-6-trifluoromethoxy-2,3-dihydropyrrolo[3,2-c]quinoline(500 mg, 1.3 mmol) was dissolved in ethanolamine(6 ml) in the pressure tube, then refluxed at 190° C. for 3 hours. The solvent was removed by distillation under reduced pressure, then the concentrate 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 380 mg of desired compound as solid in 72% of yield.

후처리

  1. customThe solvent was removed by distillation under reduced pressure
  2. additionthe concentrate 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

출처 및 근거

ORD 기록
ord-7914232b96974982ba19e67a0af7e5e2
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06011044

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