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Sodium hydride → HCID 23143999, 화합물

HRID 2357105
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HRID 2357105 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 23143999HCID 23143999, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-476b9c4594674563a154509b78a1468c
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07759470B2

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