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Sodium hydride → HCID 23143999、化合物

HRID 2357105
ノート
印刷プレビュー

反応式

HRID 2357105 の反応式
[I:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=2)[NH:4][CH:3]=1.[H-].[Na+].Cl[CH:17]1[O:21][CH:20]([CH2:22][O:23][C:24](=[O:32])[C:25]2[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][CH:26]=2)[CH:19]([O:33][C:34](=[O:42])[C:35]2[CH:40]=[CH:39][C:38]([CH3:41])=[CH:37][CH:36]=2)[CH2:18]1>C(#N)C>[I:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=2)[N:4]([CH:17]2[O:21][CH:20]([CH2:22][O:23][C:24](=[O:32])[C:25]3[CH:26]=[CH:27][C:28]([CH3:31])=[CH:29][CH:30]=3)[CH:19]([O:33][C:34](=[O:42])[C:35]3[CH:36]=[CH:37][C:38]([CH3:41])=[CH:39][CH:40]=3)[CH2:18]2)[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 2881283,5-Di-O-(p-toluyl)-2-deoxy-D-ribofuranosyl chlorideHCID 231439973-Iodo-5-nitro-1H-indole

生成物 1

HCID 23143999HCID 23143999、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 1.0 g (3.5 mmol) 3-iodo-5-nitroindole in 15 ml acetonitrile were added 0.16 g (6.7 mmol) sodium hydride (Aldrich 223441-50G). The stirring was continued and the suspension turned red. After 15 min. 2.02 g (5.2 mmol) 5-chloro-2-(4-methyl-benzoyloxymethyl)-3-(4-methyl-benzoyloxy)-tetrahydro-furan were added in small portions and the stirring was continued for another 60 minutes at room temperature. The precipitate was removed by filtration and washed once with acetonitrile. The combined yellow filtrates were concentrated until a product precipitated. For complete precipitation of the product 50 ml ethanol were added. The yellow precipitate was removed by filtration und washed with ethanol. The residuum was dried over phosphorus pentoxide and potassium hydroxide in a vacuum (yield: 1.9 g).

後処理

  1. waitthe stirring was continued for another 60 minutes at room temperature
  2. customThe precipitate was removed by filtration
  3. washwashed once with acetonitrile
  4. concentrationThe combined yellow filtrates were concentrated until a product
  5. customprecipitated
  6. customFor complete precipitation of the product 50 ml ethanol
  7. additionwere added
  8. customThe yellow precipitate was removed by filtration
  9. washund washed with ethanol
  10. dry with materialThe residuum was dried over phosphorus pentoxide and potassium hydroxide in a vacuum (yield: 1.9 g)

出典と根拠

ORDレコード
ord-476b9c4594674563a154509b78a1468c
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07759470B2

反応ノート

読み込み中…

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