Acetone → HCID 86688395、化合物

HRID 1488325ノート

反応式

HRID 1488325 の反応式
[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]

参加物

5

反応物 4

HCID 180AcetoneHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86688397HCID 86688397、化合物2 回

生成物 1

HCID 86688395HCID 86688395、化合物

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-21c3426f6aca41409c858c771a740070
出典データセット
uspto-grants-2016_08
特許番号
US09431616B2

反応ノート

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