Acetone → HCID 86688395, 화합물

HRID 1488325노트

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HRID 1488325 반응식
[P:1]1[C:14]2[CH:13]=[CH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:15]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[N:25]1[C:37]2[C:36](O)=[C:35](O)[CH:34]=[CH:33][C:32]=2[C:31]2[C:26]1=[CH:27][CH:28]=[CH:29][CH:30]=2)([CH3:18])([CH3:17])[CH3:16].[C:40](=[O:43])([O-])[O-].[K+].[K+].CI.C[C:49](C)=[O:50]>>[P:1]1[C:14]2[CH:13]=[CH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:15]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[N:25]1[C:37]2[C:36]([O:50][CH3:49])=[C:35]([O:43][CH3:40])[CH:34]=[CH:33][C:32]=2[C:31]2[C:26]1=[CH:27][CH:28]=[CH:29][CH:30]=2)([CH3:16])([CH3:17])[CH3:18]

참가 물질

5

반응물 4

HCID 180AcetoneHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86688397HCID 86688397, 화합물2회

생성물 1

HCID 86688395HCID 86688395, 화합물

실험 절차

In a 250 ml two-neck flask, N-(t-butylphenyl)dihydroxy carbazole phosphaphenanthrene (Compound I, 4.12 g), potassium carbonate (21 g), and acetone (100 ml) were mixed and stirred. Methyliodide (17.4 g) was added thereto, followed by refluxing and stirring for 1 hour. The reaction solution was filtered, and the filtrate was concentrated and dissolved in ethylacetate. The resultant was washed with distilled water, and the organic layer was dried over anhydrous magnesium sulfate. The dried organic layer was concentrated by distillation under reduced pressure and purified using a column chromatography, thereby obtaining 2 g of N-(t-butylphenyl)dimethoxy carbazole phosphaphenanthrene (Compound 201).

후처리

  1. temperatureby refluxing
  2. stirringstirring for 1 hour
  3. filtrationThe reaction solution was filtered
  4. concentrationthe filtrate was concentrated
  5. dissolutiondissolved in ethylacetate
  6. washThe resultant was washed with distilled water
  7. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  8. concentrationThe dried organic layer was concentrated by distillation under reduced pressure
  9. custompurified

출처 및 근거

ORD 기록
ord-21c3426f6aca41409c858c771a740070
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09431616B2

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