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Hydroxylamine → HCID 136337399、化合物

HRID 452130
ノート
印刷プレビュー

反応式

HRID 452130 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 787HydroxylamineHCID 1049PyridineHCID 10928Ethyl chloroformateHCID 516892Sodium BicarbonateHCID 23665647Potassium tert-butoxideHCID 67211720HCID 67211720、化合物

生成物 1

HCID 136337399HCID 136337399、化合物
収率 55%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

(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%).

後処理

  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)

出典と根拠

ORDレコード
ord-830c81fdb19f44a1b3fef8f2622e4055
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08486980B2

反応ノート

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