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Dimethylamine → HCID 22320332, 화합물

HRID 498012
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HRID 498012 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]2[N:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=3)[N:13]=[C:14]([CH3:15])[C:3]=12.[CH3:22][NH:23][CH3:24].O1CCCC1>O>[CH3:22][N:23]([CH3:24])[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]2[N:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=3)[N:13]=[C:14]([CH3:15])[C:3]=12
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참가 물질

5

반응물 3

HCID 674DimethylamineHCID 8028TetrahydrofuranHCID 223201094-Chloro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline

생성물 1

HCID 22320332HCID 22320332, 화합물수율 97%

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

4-chloro-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline (1.00 g, 3.39 mmol) was added to a 2M dimethylamine in tetrahydrofuran solution (5.00 mL, 10.0 mmol), and the solution was heated under reflux overnight at 100° C. in a sealed tube. The solution was cooled to room temperature and poured into water, and the organic matter was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and evaporated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (ethyl acetate to ethyl acetate:methanol=9:1) to give the title compound (1.00 g, 97% yield).

후처리

  1. temperaturethe solution was heated
  2. temperatureThe solution was cooled to room temperature
  3. extractionthe organic matter was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated under reduced pressure
  7. customThe residue thus obtained
  8. customwas purified by silica gel column chromatography (ethyl acetate to ethyl acetate:methanol=9:1)

출처 및 근거

ORD 기록
ord-21b50eb7fb304dc4b11ab7a273df08a0
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06949648B2

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