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Trimethylsilyl iodide → 3'',4''-Diphosphono-[2,2';5',2'';5'',2''';5''',2'''']-quinquethiophene

HRID 1662878
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HRID 1662878 반응식
C([O:3][P:4]([C:9]1[C:13]([P:14]([O:19]CC)([O:16]CC)=[O:15])=[C:12]([C:22]2[S:23][C:24]([C:27]3[S:28][CH:29]=[CH:30][CH:31]=3)=[CH:25][CH:26]=2)[S:11][C:10]=1[C:32]1[S:36][C:35]([C:37]2[S:38][CH:39]=[CH:40][CH:41]=2)=[CH:34][CH:33]=1)([O:6]CC)=[O:5])C.I[Si](C)(C)C>C(#N)C>[P:4]([C:9]1[C:13]([P:14]([OH:19])([OH:16])=[O:15])=[C:12]([C:22]2[S:23][C:24]([C:27]3[S:28][CH:29]=[CH:30][CH:31]=3)=[CH:25][CH:26]=2)[S:11][C:10]=1[C:32]1[S:36][C:35]([C:37]2[S:38][CH:39]=[CH:40][CH:41]=2)=[CH:34][CH:33]=1)([OH:5])([OH:6])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 85247Trimethylsilyl iodideHCID 591559243'',4''-Bis(diethoxyphosphoryl)-[2,2';5',2'';5'',2''';5''',2'''']-quinquethiophene

생성물 1

HCID 591558763'',4''-Diphosphono-[2,2';5',2'';5'',2''';5''',2'''']-quinquethiophene수율 71%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

In 4.0 ml of acetonitrile, 0.2746 g (0.401 mmols) of 3″,4″-bis(diethoxyphosphoryl)-[2,2′;5′,2″;5″,2″′;5″′,2″″]-quinquethiophene was dissolved, to which 0.4012 g (2.005 mmols) of commercially available iodotrimethylsilane was added at room temperature. Thereafter, the mixture was stirred at room temperature for 12 hours. After the reaction, the solvent was removed by distilling off under reduced pressure, followed by addition of methanol and stirring at room temperature for further 12 hours. A sodium thiosulfate aqueous solution was added, followed by stirring, filtration of the precipitated crystals, washing with distilled water, methanol, chloroform and diethyl ether and drying to obtain the specified substance in the form of a yellow powder at a yield of 0.1630 g (yield: 71%).

후처리

  1. additionwas added at room temperature
  2. customAfter the reaction
  3. customthe solvent was removed
  4. distillationby distilling off under reduced pressure
  5. additionfollowed by addition of methanol
  6. stirringstirring at room temperature for further 12 hours
  7. additionA sodium thiosulfate aqueous solution was added
  8. stirringby stirring
  9. filtrationfiltration of the precipitated crystals
  10. washwashing with distilled water, methanol, chloroform and diethyl ether
  11. customdrying
  12. customto obtain the specified substance in the form of a yellow powder at a yield of 0.1630 g (yield: 71%)

출처 및 근거

ORD 기록
ord-b05147d46ffb4d2ba5172cda13223006
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030438B2

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