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2-Butanamine, 2-methyl- → 6,7-dichloro-2,3-dimethoxy-5-{[2-(N-(1,1-dimethylpropyl)amino)ethyl]pyrazol-1-ylmethyl}quinoxaline

HRID 1957114
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HRID 1957114 반응식
Cl[CH2:2][CH2:3][CH:4]([N:21]1[CH:25]=[CH:24][CH:23]=[N:22]1)[C:5]1[C:14]([Cl:15])=[C:13]([Cl:16])[CH:12]=[C:11]2[C:6]=1[N:7]=[C:8]([O:19][CH3:20])[C:9]([O:17][CH3:18])=[N:10]2.[CH3:26][C:27]([NH2:31])([CH3:30])[CH2:28][CH3:29]>C(O)C>[Cl:15][C:14]1[C:5]([CH:4]([CH2:3][CH2:2][NH:31][C:27]([CH3:30])([CH3:26])[CH2:28][CH3:29])[N:21]2[CH:25]=[CH:24][CH:23]=[N:22]2)=[C:6]2[C:11](=[CH:12][C:13]=1[Cl:16])[N:10]=[C:9]([O:17][CH3:18])[C:8]([O:19][CH3:20])=[N:7]2
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참가 물질

4

반응물 2

HCID 689862-Butanamine, 2-methyl-HCID 543391965-[(2-Chloroethyl)pyrazol-1-ylmethyl]-6,7-dichloro-2,3-dimethoxyquinoxaline

생성물 1

HCID 232249886,7-dichloro-2,3-dimethoxy-5-{[2-(N-(1,1-dimethylpropyl)amino)ethyl]pyrazol-1-ylmethyl}quinoxaline수율 38%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
105 °C

실험 절차

A mixture of 5-[(2-chloroethyl)pyrazol-1-ylmethyl]-6,7-dichloro-2,3-dimethoxyquinoxaline (150 mg, 0.37 mmol), 1,1-dimethyl-1-propylamine (3 mL) and ethanol (5 mL) were heated in a closed vessel at 105° C. for 7 hours. The mixture was cooled, the solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate (75 mL). The solution was washed with saturated aqueous sodium bicarbonate, dried (MgSO4) and concentrated under reduced pressure. Purification by flash chromatography (elution with dichloromethane, then an ethyl acetate/methanol/triethylamine gradient) gave 6,7-dichloro-2,3-dimethoxy-5-{[2-(N-(1,1-dimethylpropyl)amino)ethyl]pyrazol-1-ylmethyl}quinoxaline (65 mg, 38%), as a pale yellow solid.

후처리

  1. temperatureThe mixture was cooled
  2. customthe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate (75 mL)
  4. washThe solution was washed with saturated aqueous sodium bicarbonate
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure
  7. customPurification by flash chromatography (
  8. washelution with dichloromethane

출처 및 근거

ORD 기록
ord-7e8695b6787e4c51a6b28f32700ac456
출처 데이터셋
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05783572

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