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Hydroxylamine → HCID 136337399, 화합물

HRID 452130
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HRID 452130 반응식
[CH2:1]([C:4]1[N:8]([CH2:9][C:10]2[CH:27]=[CH:26][C:13]3/[C:14](=[CH:23]/[C:24]#[N:25])/[C:15]4[CH:22]=[CH:21][CH:20]=[CH:19][C:16]=4[CH2:17][CH2:18][C:12]=3[CH:11]=2)[C:7]2[CH:28]=[CH:29][CH:30]=[CH:31][C:6]=2[N:5]=1)[CH2:2][CH3:3].NO.[N:34]1C=CC=CC=1.[C:40](Cl)(=[O:44])[O:41]CC.C(=O)([O-])O.[Na+].CC(C)([O-])C.[K+]>C(O)C.C(OCC)(=O)C>[CH2:1]([C:4]1[N:8]([CH2:9][C:10]2[CH:27]=[CH:26][C:13]3/[C:14](=[CH:23]/[C:24]4[NH:34][C:40](=[O:44])[O:41][N:25]=4)/[C:15]4[CH:22]=[CH:21][CH:20]=[CH:19][C:16]=4[CH2:17][CH2:18][C:12]=3[CH:11]=2)[C:7]2[CH:28]=[CH:29][CH:30]=[CH:31][C:6]=2[N:5]=1)[CH2:2][CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 787HydroxylamineHCID 1049PyridineHCID 10928Ethyl chloroformateHCID 516892Sodium BicarbonateHCID 23665647Potassium tert-butoxideHCID 67211720HCID 67211720, 화합물

생성물 1

HCID 136337399HCID 136337399, 화합물
수율 55%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매2회

실험 절차

(E)-[2-(2-Propylbenzimidazol-1-yl)methyl-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene]acetonitrile (467 mg, 1.16 mmol) obtained in Example 1 was dissolved in ethanol (11 mL), hydroxylamine (50% aqueous solution, 2.13 mL, 34.7 mmol) was added, and the mixture was heated under reflux for 16 hr, and concentrated under reduced pressure. The obtained residue was dissolved in DMF (5.5 mL), pyridine (112 μL, 1.39 mmol) and ethyl chlorocarbonate (133 μL, 1.39 mmol) were added at 0° C., and the mixture was stirred at room temperature for 1 hr. Ethyl acetate and saturated aqueous sodium hydrogen carbonate solution were added to the mixture. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was dissolved in toluene (11 mL), potassium tert-butoxide (195 mg, 1.74 mmol) was added, and the mixture was stirred at room temperature for 15 min. Ethyl acetate was added to the mixture, and the organic layer was washed with 5% aqueous citric acid solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol=99/1) to give the title compound (compound 5) (295 mg, 55%).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 16 hr
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe obtained residue was dissolved in DMF (5.5 mL)
  5. washThe organic layer was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. dissolutionThe obtained residue was dissolved in toluene (11 mL)
  9. stirringthe mixture was stirred at room temperature for 15 min
  10. washthe organic layer was washed with 5% aqueous citric acid solution
  11. dry with materialdried over anhydrous magnesium sulfate
  12. concentrationconcentrated under reduced pressure
  13. customThe residue was purified by silica gel column chromatography (chloroform/methanol=99/1)

출처 및 근거

ORD 기록
ord-830c81fdb19f44a1b3fef8f2622e4055
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486980B2

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